Spontaneous Electronic Band Formation and Switchable Behaviors in a Phase-Rich Superatomic Crystal.
O'Brien, Evan S; Russell, Jake C.; Bartnof, Matthew; Christodoulides, Alexander D.; Lee, Kihong; DeGayner, Jordan A.; Paley, Daniel W.; McGaughey, Alan J. H.; Ong, Wee-Liat; Malen, Jonathan A.; Zhu, X.-Y.; Roy, Xavier; Journal of the American Chemical Society 140 (2018) 15601–15605; doi:10.1021/jacs.8b09905

data_4133410
_publ_section_title
;
 Spontaneous Electronic Band Formation and Switchable Behaviors in a
 Phase-Rich Superatomic Crystal.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15601
_journal_page_last               15605
_journal_paper_doi               10.1021/jacs.8b09905
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C36 H90 Co6 P6 Te8), 2(C70), C140'
_chemical_formula_sum            'C352 H180 Co12 P12 Te16'
_chemical_formula_weight         7529.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.161(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.7743(9)
_cell_length_b                   16.3541(5)
_cell_length_c                   28.9052(10)
_cell_measurement_reflns_used    11974
_cell_measurement_temperature    250.2(3)
_cell_measurement_theta_max      28.8540
_cell_measurement_theta_min      3.9510
_cell_volume                     12175.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      250.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -29.00  51.00   0.50    2.00    --  -14.01  57.00  90.00  160
  2  \w     26.00  81.00   0.50    2.00    --   16.51  57.00 -30.00  110
  3  \w     -8.00  83.00   0.50    2.00    --   16.51  77.00-150.00  182
  4  \w     36.00  63.00   0.50    2.00    --   16.51 178.00-180.00   54
  5  \w    -79.00 -31.00   0.50    2.00    --  -14.01 -37.00 120.00   96
  6  \w    -57.00 -31.00   0.50    2.00    --  -14.01 -77.00  60.00   52
  7  \w    -25.00   9.00   0.50    2.00    --  -14.01 -77.00  60.00   68
  8  \w    -12.00  53.00   0.50    2.00    --   16.51 -99.00  30.00  130
  9  \w    -42.00  -8.00   0.50    2.00    --  -14.01 -57.00-120.00   68
 10  \w    -80.00 -54.00   0.50    2.00    --  -14.01 -77.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0122336000
_diffrn_orient_matrix_UB_12      0.0187060000
_diffrn_orient_matrix_UB_13      0.0188270000
_diffrn_orient_matrix_UB_21      0.0208362000
_diffrn_orient_matrix_UB_22      -0.0124895000
_diffrn_orient_matrix_UB_23      0.0151119000
_diffrn_orient_matrix_UB_31      0.0131864000
_diffrn_orient_matrix_UB_32      0.0371265000
_diffrn_orient_matrix_UB_33      -0.0044433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            59639
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       block
_exptl_crystal_F_000             7256
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1447
_refine_ls_number_reflns         12880
_refine_ls_number_restraints     4674
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+68.3570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7485
_reflns_number_total             12880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09905_si_003.cif
_cod_data_source_block           CoTe-C70-250
_cod_database_code               4133410
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C176 H90 Co6 Te8 P6'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-C66 \\sim C15A-C16A \\sim C55-C56 \\sim C15B-C16B \\sim C45-C46 \\sim
C25-C26 \\sim C35-C36
 with sigma of 0.02
 P1-C13B \\sim P1-C13A \\sim P5-C53 \\sim P2-C23 \\sim P4-C43 \\sim P6-C63
\\sim P3-C33
 with sigma of 0.02
 P6-C65 \\sim P1-C15A \\sim P5-C55 \\sim P4-C45 \\sim P2-C25 \\sim P1-C15B
\\sim P3-C35
 with sigma of 0.02
 P2-C21 \\sim P1-C11A \\sim P5-C51 \\sim P6-C61 \\sim P1-C11B \\sim P4-C41
\\sim P3-C31
 with sigma of 0.02
 C63-C64 \\sim C13A-C14A \\sim C23-C24 \\sim C53-C54 \\sim C43-C44 \\sim
C13B-C14B \\sim C33-C34
 with sigma of 0.02
 C41-C42 \\sim C11A-C12A \\sim C11B-C12B \\sim C21-C22 \\sim C31-C32 \\sim
C61-C62 \\sim C51-C52
 with sigma of 0.02
 Co3-P3 \\sim Co1-P1 \\sim Co6-P6 \\sim Co2-P2 \\sim Co5-P5 \\sim Co4-P4
 with sigma of 0.02
 P3-C34 \\sim P1-C14A \\sim P4-C44 \\sim P2-C24 \\sim P5-C54 \\sim P1-C14B
\\sim P6-C64
 with sigma of 0.04
 Co3-C33 \\sim Co1-C13A \\sim Co4-C43 \\sim Co2-C23 \\sim Co5-C53 \\sim Co6-C63
\\sim Co1-C13B
 with sigma of 0.04
 P3-C32 \\sim P1-C12A \\sim P5-C52 \\sim P2-C22 \\sim P6-C62 \\sim P4-C42 \\sim
P1-C12B
 with sigma of 0.04
 Co2-C25 \\sim Co1-C15A \\sim Co5-C55 \\sim Co1-C15B \\sim Co3-C35 \\sim
Co4-C45 \\sim Co6-C65
 with sigma of 0.04
 Co5-C51 \\sim Co1-C11A \\sim Co4-C41 \\sim Co3-C31 \\sim Co2-C21 \\sim Co6-C61
\\sim Co1-C11B
 with sigma of 0.04
 C51-C53 \\sim C11A-C13A \\sim C11B-C13B \\sim C61-C63 \\sim C31-C33 \\sim
C21-C23 \\sim C41-C43
 with sigma of 0.04
 C53-C55 \\sim C13A-C15A \\sim C43-C45 \\sim C23-C25 \\sim C33-C35 \\sim
C13B-C15B \\sim C63-C65
 with sigma of 0.04
 P4-C46 \\sim P1-C16A \\sim P2-C26 \\sim P1-C16B \\sim P3-C36 \\sim P5-C56
\\sim P6-C66
 with sigma of 0.04
 C41-C45 \\sim C11A-C15A \\sim C11B-C15B \\sim C51-C55 \\sim C61-C65 \\sim
C21-C25 \\sim C31-C35
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1_1) \\sim Ueq, Uanis(C2_1) \\sim Ueq, Uanis(C3_1) \\sim Ueq,
Uanis(C4_1) \\sim Ueq, Uanis(C5_1) \\sim Ueq, Uanis(C6_1) \\sim Ueq,
Uanis(C7_1) \\sim Ueq, Uanis(C8_1) \\sim Ueq, Uanis(C9_1) \\sim Ueq,
Uanis(C10_1) \\sim Ueq, Uanis(C11_1) \\sim Ueq, Uanis(C12_1) \\sim Ueq,
Uanis(C13_1) \\sim Ueq, Uanis(C14_1) \\sim Ueq, Uanis(C15_1) \\sim Ueq,
Uanis(C16_1) \\sim Ueq, Uanis(C17_1) \\sim Ueq, Uanis(C18_1) \\sim Ueq,
Uanis(C19_1) \\sim Ueq, Uanis(C20_1) \\sim Ueq, Uanis(C21_1) \\sim Ueq,
Uanis(C22_1) \\sim Ueq, Uanis(C23_1) \\sim Ueq, Uanis(C24_1) \\sim Ueq,
Uanis(C25_1) \\sim Ueq, Uanis(C26_1) \\sim Ueq, Uanis(C27_1) \\sim Ueq,
Uanis(C28_1) \\sim Ueq, Uanis(C29_1) \\sim Ueq, Uanis(C30_1) \\sim Ueq,
Uanis(C31_1) \\sim Ueq, Uanis(C32_1) \\sim Ueq, Uanis(C33_1) \\sim Ueq,
Uanis(C34_1) \\sim Ueq, Uanis(C35_1) \\sim Ueq, Uanis(C36_1) \\sim Ueq,
Uanis(C37_1) \\sim Ueq, Uanis(C38_1) \\sim Ueq, Uanis(C39_1) \\sim Ueq,
Uanis(C40_1) \\sim Ueq, Uanis(C41_1) \\sim Ueq, Uanis(C42_1) \\sim Ueq,
Uanis(C43_1) \\sim Ueq, Uanis(C44_1) \\sim Ueq, Uanis(C45_1) \\sim Ueq,
Uanis(C46_1) \\sim Ueq, Uanis(C47_1) \\sim Ueq, Uanis(C48_1) \\sim Ueq,
Uanis(C49_1) \\sim Ueq, Uanis(C50_1) \\sim Ueq, Uanis(C51_1) \\sim Ueq,
Uanis(C52_1) \\sim Ueq, Uanis(C53_1) \\sim Ueq, Uanis(C54_1) \\sim Ueq,
Uanis(C55_1) \\sim Ueq, Uanis(C56_1) \\sim Ueq, Uanis(C57_1) \\sim Ueq,
Uanis(C58_1) \\sim Ueq, Uanis(C59_1) \\sim Ueq, Uanis(C60_1) \\sim Ueq,
Uanis(C61_1) \\sim Ueq, Uanis(C62_1) \\sim Ueq, Uanis(C63_1) \\sim Ueq,
Uanis(C64_1) \\sim Ueq, Uanis(C65_1) \\sim Ueq, Uanis(C66_1) \\sim Ueq,
Uanis(C67_1) \\sim Ueq, Uanis(C68_1) \\sim Ueq, Uanis(C69_1) \\sim Ueq,
Uanis(C70_1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1_2) \\sim Ueq, Uanis(C2_2) \\sim Ueq, Uanis(C3_2) \\sim Ueq,
Uanis(C4_2) \\sim Ueq, Uanis(C5_2) \\sim Ueq, Uanis(C6_2) \\sim Ueq,
Uanis(C7_2) \\sim Ueq, Uanis(C8_2) \\sim Ueq, Uanis(C9_2) \\sim Ueq,
Uanis(C10_2) \\sim Ueq, Uanis(C11_2) \\sim Ueq, Uanis(C12_2) \\sim Ueq,
Uanis(C13_2) \\sim Ueq, Uanis(C14_2) \\sim Ueq, Uanis(C15_2) \\sim Ueq,
Uanis(C16_2) \\sim Ueq, Uanis(C17_2) \\sim Ueq, Uanis(C18_2) \\sim Ueq,
Uanis(C19_2) \\sim Ueq, Uanis(C20_2) \\sim Ueq, Uanis(C21_2) \\sim Ueq,
Uanis(C22_2) \\sim Ueq, Uanis(C23_2) \\sim Ueq, Uanis(C24_2) \\sim Ueq,
Uanis(C25_2) \\sim Ueq, Uanis(C26_2) \\sim Ueq, Uanis(C27_2) \\sim Ueq,
Uanis(C28_2) \\sim Ueq, Uanis(C29_2) \\sim Ueq, Uanis(C30_2) \\sim Ueq,
Uanis(C31_2) \\sim Ueq, Uanis(C32_2) \\sim Ueq, Uanis(C33_2) \\sim Ueq,
Uanis(C34_2) \\sim Ueq, Uanis(C35_2) \\sim Ueq, Uanis(C36_2) \\sim Ueq,
Uanis(C37_2) \\sim Ueq, Uanis(C38_2) \\sim Ueq, Uanis(C39_2) \\sim Ueq,
Uanis(C40_2) \\sim Ueq, Uanis(C41_2) \\sim Ueq, Uanis(C42_2) \\sim Ueq,
Uanis(C43_2) \\sim Ueq, Uanis(C44_2) \\sim Ueq, Uanis(C45_2) \\sim Ueq,
Uanis(C46_2) \\sim Ueq, Uanis(C47_2) \\sim Ueq, Uanis(C48_2) \\sim Ueq,
Uanis(C49_2) \\sim Ueq, Uanis(C50_2) \\sim Ueq, Uanis(C51_2) \\sim Ueq,
Uanis(C52_2) \\sim Ueq, Uanis(C53_2) \\sim Ueq, Uanis(C54_2) \\sim Ueq,
Uanis(C55_2) \\sim Ueq, Uanis(C56_2) \\sim Ueq, Uanis(C57_2) \\sim Ueq,
Uanis(C58_2) \\sim Ueq, Uanis(C59_2) \\sim Ueq, Uanis(C60_2) \\sim Ueq,
Uanis(C61_2) \\sim Ueq, Uanis(C62_2) \\sim Ueq, Uanis(C63_2) \\sim Ueq,
Uanis(C64_2) \\sim Ueq, Uanis(C65_2) \\sim Ueq, Uanis(C66_2) \\sim Ueq,
Uanis(C67_2) \\sim Ueq, Uanis(C68_2) \\sim Ueq, Uanis(C69_2) \\sim Ueq,
Uanis(C70_2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C11A, C12A, C13A, C14A, C15A, C16A, C11B, C12B, C13B, C14B, C15B, C16B, C21,
 C22, C23, C24, C25, C26, C31, C32, C33, C34, C35, C36, C41, C42, C43, C44, C45,
  C46, C51, C52, C53, C54, C55, C56, C61, C62, C63, C64, C65, C66, P1, P2, P3,
 P4, P5, P6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1, C9_1, C10_1, C11_1, C12_1,
 C13_1, C14_1, C15_1, C16_1, C17_1, C18_1, C19_1, C20_1, C21_1, C22_1, C23_1,
 C24_1, C25_1, C26_1, C27_1, C28_1, C29_1, C30_1, C31_1, C32_1, C33_1, C34_1,
 C35_1, C36_1, C37_1, C38_1, C39_1, C40_1, C41_1, C42_1, C43_1, C44_1, C45_1,
 C46_1, C47_1, C48_1, C49_1, C50_1, C51_1, C52_1, C53_1, C54_1, C55_1, C56_1,
 C57_1, C58_1, C59_1, C60_1, C61_1, C62_1, C63_1, C64_1, C65_1, C66_1, C67_1,
 C68_1, C69_1, C70_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2, C9_2, C10_2, C11_2, C12_2,
 C13_2, C14_2, C15_2, C16_2, C17_2, C18_2, C19_2, C20_2, C21_2, C22_2, C23_2,
 C24_2, C25_2, C26_2, C27_2, C28_2, C29_2, C30_2, C31_2, C32_2, C33_2, C34_2,
 C35_2, C36_2, C37_2, C38_2, C39_2, C40_2, C41_2, C42_2, C43_2, C44_2, C45_2,
 C46_2, C47_2, C48_2, C49_2, C50_2, C51_2, C52_2, C53_2, C54_2, C55_2, C56_2,
 C57_2, C58_2, C59_2, C60_2, C61_2, C62_2, C63_2, C64_2, C65_2, C66_2, C67_2,
 C68_2, C69_2, C70_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Co1, P1, C11B, C12B, C13B, C14B, C15B, C16B} sigma for 1-2: 0.02, 1-3: 0.04
{Co2, P2, C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{Co3, P3, C31, C32, C33, C34, C35, C36} sigma for 1-2: 0.02, 1-3: 0.04
{Co4, P4, C41, C42, C43, C44, C45, C46} sigma for 1-2: 0.02, 1-3: 0.04
{Co5, P5, C51, C52, C53, C54, C55, C56} sigma for 1-2: 0.02, 1-3: 0.04
{Co6, P6, C61, C62, C63, C64, C65, C66} sigma for 1-2: 0.02, 1-3: 0.04
as
{Co1, P1, C11A, C12A, C13A, C14A, C15A, C16A}
6. Others
 1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+Sof(C8)+Sof(C9)+
 Sof(C10)+Sof(C11)+Sof(C12)+Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+Sof(C17)+
 Sof(C18)+Sof(C19)+Sof(C20)+Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+Sof(C25)+
 Sof(C26)+Sof(C27)+Sof(C28)+Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+Sof(C33)+
 Sof(C34)+Sof(C35)+Sof(C36)+Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+Sof(C41)+
 Sof(C42)+Sof(C43)+Sof(C44)+Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+Sof(C49)+
 Sof(C50)+Sof(C51)+Sof(C52)+Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+Sof(C57)+
 Sof(C58)+Sof(C59)+Sof(C60)+Sof(C61)+Sof(C62)+Sof(C63)+Sof(C64)+Sof(C65)+
 Sof(C66)+Sof(C67)+Sof(C68)+Sof(C69)+Sof(C70)]+1*[Sof(C1)+Sof(C2)+Sof(C3)+
 Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+Sof(C8)+Sof(C9)+Sof(C10)+Sof(C11)+Sof(C12)+
 Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+Sof(C17)+Sof(C18)+Sof(C19)+Sof(C20)+
 Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+Sof(C25)+Sof(C26)+Sof(C27)+Sof(C28)+
 Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+Sof(C33)+Sof(C34)+Sof(C35)+Sof(C36)+
 Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+Sof(C41)+Sof(C42)+Sof(C43)+Sof(C44)+
 Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+Sof(C49)+Sof(C50)+Sof(C51)+Sof(C52)+
 Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+Sof(C57)+Sof(C58)+Sof(C59)+Sof(C60)+
 Sof(C61)+Sof(C62)+Sof(C63)+Sof(C64)+Sof(C65)+Sof(C66)+Sof(C67)+Sof(C68)+
 Sof(C69)+Sof(C70)]+1*[Sof(C1)+Sof(C2)+Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+
 Sof(C8)+Sof(C9)+Sof(C10)+Sof(C11)+Sof(C12)+Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+
 Sof(C17)+Sof(C18)+Sof(C19)+Sof(C20)+Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+
 Sof(C25)+Sof(C26)+Sof(C27)+Sof(C28)+Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+
 Sof(C33)+Sof(C34)+Sof(C35)+Sof(C36)+Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+
 Sof(C41)+Sof(C42)+Sof(C43)+Sof(C44)+Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+
 Sof(C49)+Sof(C50)+Sof(C51)+Sof(C52)+Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+
 Sof(C57)+Sof(C58)+Sof(C59)+Sof(C60)+Sof(C61)+Sof(C62)+Sof(C63)+Sof(C64)+
 Sof(C65)+Sof(C66)+Sof(C67)+Sof(C68)+Sof(C69)+Sof(C70)]+1*[Sof(C1)+Sof(C2)+
 Sof(C3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(C7)+Sof(C8)+Sof(C9)+Sof(C10)+Sof(C11)+
 Sof(C12)+Sof(C13)+Sof(C14)+Sof(C15)+Sof(C16)+Sof(C17)+Sof(C18)+Sof(C19)+
 Sof(C20)+Sof(C21)+Sof(C22)+Sof(C23)+Sof(C24)+Sof(C25)+Sof(C26)+Sof(C27)+
 Sof(C28)+Sof(C29)+Sof(C30)+Sof(C31)+Sof(C32)+Sof(C33)+Sof(C34)+Sof(C35)+
 Sof(C36)+Sof(C37)+Sof(C38)+Sof(C39)+Sof(C40)+Sof(C41)+Sof(C42)+Sof(C43)+
 Sof(C44)+Sof(C45)+Sof(C46)+Sof(C47)+Sof(C48)+Sof(C49)+Sof(C50)+Sof(C51)+
 Sof(C52)+Sof(C53)+Sof(C54)+Sof(C55)+Sof(C56)+Sof(C57)+Sof(C58)+Sof(C59)+
 Sof(C60)+Sof(C61)+Sof(C62)+Sof(C63)+Sof(C64)+Sof(C65)+Sof(C66)+Sof(C67)+
 Sof(C68)+Sof(C69)+Sof(C70)]=1 with esd of 0.0002
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*(1-FVAR(2))
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*FVAR(2)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*FVAR(3)
 Uiso(C1)=Uiso(C2)=Uiso(C3)=Uiso(C4)=Uiso(C5)=Uiso(C6)=Uiso(C7)=Uiso(C8)=
 Uiso(C9)=Uiso(C10)=Uiso(C11)=Uiso(C12)=Uiso(C13)=Uiso(C14)=Uiso(C15)=Uiso(C16)=
 Uiso(C17)=Uiso(C18)=Uiso(C19)=Uiso(C20)=Uiso(C21)=Uiso(C22)=Uiso(C23)=
 Uiso(C24)=Uiso(C25)=Uiso(C26)=Uiso(C27)=Uiso(C28)=Uiso(C29)=Uiso(C30)=
 Uiso(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=Uiso(C37)=
 Uiso(C38)=Uiso(C39)=Uiso(C40)=Uiso(C41)=Uiso(C42)=Uiso(C43)=Uiso(C44)=
 Uiso(C45)=Uiso(C46)=Uiso(C47)=Uiso(C48)=Uiso(C49)=Uiso(C50)=Uiso(C51)=
 Uiso(C52)=Uiso(C53)=Uiso(C54)=Uiso(C55)=Uiso(C56)=Uiso(C57)=Uiso(C58)=
 Uiso(C59)=Uiso(C60)=Uiso(C61)=Uiso(C62)=Uiso(C63)=Uiso(C64)=Uiso(C65)=
 Uiso(C66)=Uiso(C67)=Uiso(C68)=Uiso(C69)=Uiso(C70)=FVAR(3)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*FVAR(5)
 Uiso(C1)=Uiso(C2)=Uiso(C3)=Uiso(C4)=Uiso(C5)=Uiso(C6)=Uiso(C7)=Uiso(C8)=
 Uiso(C9)=Uiso(C10)=Uiso(C11)=Uiso(C12)=Uiso(C13)=Uiso(C14)=Uiso(C15)=Uiso(C16)=
 Uiso(C17)=Uiso(C18)=Uiso(C19)=Uiso(C20)=Uiso(C21)=Uiso(C22)=Uiso(C23)=
 Uiso(C24)=Uiso(C25)=Uiso(C26)=Uiso(C27)=Uiso(C28)=Uiso(C29)=Uiso(C30)=
 Uiso(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=Uiso(C37)=
 Uiso(C38)=Uiso(C39)=Uiso(C40)=Uiso(C41)=Uiso(C42)=Uiso(C43)=Uiso(C44)=
 Uiso(C45)=Uiso(C46)=Uiso(C47)=Uiso(C48)=Uiso(C49)=Uiso(C50)=Uiso(C51)=
 Uiso(C52)=Uiso(C53)=Uiso(C54)=Uiso(C55)=Uiso(C56)=Uiso(C57)=Uiso(C58)=
 Uiso(C59)=Uiso(C60)=Uiso(C61)=Uiso(C62)=Uiso(C63)=Uiso(C64)=Uiso(C65)=
 Uiso(C66)=Uiso(C67)=Uiso(C68)=Uiso(C69)=Uiso(C70)=FVAR(5)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*FVAR(7)
 Uiso(C1)=Uiso(C2)=Uiso(C3)=Uiso(C4)=Uiso(C5)=Uiso(C6)=Uiso(C7)=Uiso(C8)=
 Uiso(C9)=Uiso(C10)=Uiso(C11)=Uiso(C12)=Uiso(C13)=Uiso(C14)=Uiso(C15)=Uiso(C16)=
 Uiso(C17)=Uiso(C18)=Uiso(C19)=Uiso(C20)=Uiso(C21)=Uiso(C22)=Uiso(C23)=
 Uiso(C24)=Uiso(C25)=Uiso(C26)=Uiso(C27)=Uiso(C28)=Uiso(C29)=Uiso(C30)=
 Uiso(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=Uiso(C37)=
 Uiso(C38)=Uiso(C39)=Uiso(C40)=Uiso(C41)=Uiso(C42)=Uiso(C43)=Uiso(C44)=
 Uiso(C45)=Uiso(C46)=Uiso(C47)=Uiso(C48)=Uiso(C49)=Uiso(C50)=Uiso(C51)=
 Uiso(C52)=Uiso(C53)=Uiso(C54)=Uiso(C55)=Uiso(C56)=Uiso(C57)=Uiso(C58)=
 Uiso(C59)=Uiso(C60)=Uiso(C61)=Uiso(C62)=Uiso(C63)=Uiso(C64)=Uiso(C65)=
 Uiso(C66)=Uiso(C67)=Uiso(C68)=Uiso(C69)=Uiso(C70)=FVAR(7)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(C9)=
 Sof(C10)=Sof(C11)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(C26)=Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=
 Sof(C34)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(C39)=Sof(C40)=Sof(C41)=
 Sof(C42)=Sof(C43)=Sof(C44)=Sof(C45)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=
 Sof(C50)=Sof(C51)=Sof(C52)=Sof(C53)=Sof(C54)=Sof(C55)=Sof(C56)=Sof(C57)=
 Sof(C58)=Sof(C59)=Sof(C60)=Sof(C61)=Sof(C62)=Sof(C63)=Sof(C64)=Sof(C65)=
 Sof(C66)=Sof(C67)=Sof(C68)=Sof(C69)=Sof(C70)=0.5*FVAR(9)
 Uiso(C1)=Uiso(C2)=Uiso(C3)=Uiso(C4)=Uiso(C5)=Uiso(C6)=Uiso(C7)=Uiso(C8)=
 Uiso(C9)=Uiso(C10)=Uiso(C11)=Uiso(C12)=Uiso(C13)=Uiso(C14)=Uiso(C15)=Uiso(C16)=
 Uiso(C17)=Uiso(C18)=Uiso(C19)=Uiso(C20)=Uiso(C21)=Uiso(C22)=Uiso(C23)=
 Uiso(C24)=Uiso(C25)=Uiso(C26)=Uiso(C27)=Uiso(C28)=Uiso(C29)=Uiso(C30)=
 Uiso(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=Uiso(C37)=
 Uiso(C38)=Uiso(C39)=Uiso(C40)=Uiso(C41)=Uiso(C42)=Uiso(C43)=Uiso(C44)=
 Uiso(C45)=Uiso(C46)=Uiso(C47)=Uiso(C48)=Uiso(C49)=Uiso(C50)=Uiso(C51)=
 Uiso(C52)=Uiso(C53)=Uiso(C54)=Uiso(C55)=Uiso(C56)=Uiso(C57)=Uiso(C58)=
 Uiso(C59)=Uiso(C60)=Uiso(C61)=Uiso(C62)=Uiso(C63)=Uiso(C64)=Uiso(C65)=
 Uiso(C66)=Uiso(C67)=Uiso(C68)=Uiso(C69)=Uiso(C70)=FVAR(9)
 Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=0.5*(1-
 FVAR(11))
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=0.5*
 FVAR(11)
 Fixed Sof: Te1(0.5) Te2(0.5) Te3(0.5) Te4(0.5) Te5(0.5) Te7(0.5) Te8(0.5)
 Co1(0.5) P1(0.5) Co2(0.5) P2(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) C24(0.5) H24A(0.5)
 H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5)
 H26C(0.5) Co3(0.5) P3(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
 Co4(0.5) P4(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C45(0.5) H45A(0.5) H45B(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) Co5(0.5)
 P5(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5)
 H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) Co6(0.5) P6(0.5)
 C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5) H65A(0.5)
 H65B(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5)
7.a Free rotating group:
 C1(C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,
 C22,C23,C24,C25,C26,C27,C28,C29,C30,C31,C32,C33,C34,C35,C36,C37,C38,C39,C40,
 C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,C51,C52,C53,C54,C55,C56,C57,C58,C59,
 C60,C61,C62,C63,C64,C65,C66,C67,C68,C69,C70)
7.b Secondary CH2 refined with riding coordinates:
 C11A(H11A,H11B), C13A(H13A,H13B), C15A(H15A,H15B), C11B(H11C,H11D), C13B(H13C,
 H13D), C15B(H15C,H15D), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B),
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C41(H41A,H41B), C43(H43A,H43B),
  C45(H45A,H45B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,H55B), C61(H61A,
 H61B), C63(H63A,H63B), C65(H65A,H65B)
7.c Me refined with riding coordinates:
 C12A(H12A,H12B,H12C), C14A(H14A,H14B,H14C), C16A(H16A,H16B,H16C), C12B(H12D,
 H12E,H12F), C14B(H14D,H14E,H14F), C16B(H16D,H16E,H16F), C22(H22A,H22B,H22C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              56863
_shelx_hkl_checksum              9373
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.876
_oxdiff_exptl_absorpt_empirical_full_min 0.569