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_4133412
_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         'C36 H90 Co6 P6 Te8, 2(C70)'
_chemical_formula_sum            'C176 H90 Co6 P6 Te8'
_chemical_formula_weight         3764.67
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   16.6030(8)
_cell_length_b                   16.6030(8)
_cell_length_c                   12.9455(9)
_cell_measurement_reflns_used    8645
_cell_measurement_temperature    340.3(4)
_cell_measurement_theta_max      28.2860
_cell_measurement_theta_min      3.9810
_cell_volume                     3090.5(3)
_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      air
_diffrn_ambient_temperature      340.3(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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     18.00  60.00   1.00    5.00    --   16.51-110.00  15.00   42
  2  \w     50.00  76.00   1.00    5.00    --   16.51   0.00 -90.00   26
  3  \w     11.00  52.00   1.00    5.00    --  -14.01  57.00-150.00   41
  4  \w    -29.00   1.00   1.00    5.00    --  -14.01 -57.00  90.00   30
  5  \w    -40.00  -7.00   1.00    5.00    --  -14.01 -37.00  30.00   33
  6  \w    -53.00  42.00   1.00    5.00    --   16.51   0.00 -90.00   95
  7  \w      5.00  31.00   1.00    5.00    --  -14.01  57.00 -90.00   26
  8  \w     -9.00  82.00   1.00    5.00    --   16.51  77.00-120.00   91
  9  \w      2.00  76.00   1.00    5.00    --   16.51  57.00 120.00   74
;
_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      -0.0127406000
_diffrn_orient_matrix_UB_12      -0.0227030000
_diffrn_orient_matrix_UB_13      0.0485927000
_diffrn_orient_matrix_UB_21      -0.0106783000
_diffrn_orient_matrix_UB_22      -0.0425875000
_diffrn_orient_matrix_UB_23      -0.0240742000
_diffrn_orient_matrix_UB_31      0.0464488000
_diffrn_orient_matrix_UB_32      0.0101556000
_diffrn_orient_matrix_UB_33      0.0078220000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.399
_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    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2342
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+9.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1869
_reflns_number_total             2342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09905_si_002.cif
_cod_data_source_block           CoTe-C70-340
_cod_original_cell_volume        3090.4(4)
_cod_database_code               4133412
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co6 Te8 P6 C176 H90'
_reflns_odcompleteness_completeness 99.57
_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
 C1-C2 = C3-C4 = C5-C6
 1.54 with sigma of 0.02
 P1-C1 = P1-C3 = P1-C5
 1.82 with sigma of 0.02
 P1-C2 = P1-C4 = P1-C6
 2.85 with sigma of 0.04
3. Rigid body (RIGU) restrains
 P1, C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 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(1)
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C1(0.16667) C2(0.16667)
 C3(0.16667) C4(0.16667) C5(0.16667) C6(0.16667) C7(0.16667) C8(0.16667)
 C9(0.16667) C10(0.16667) C11(0.16667) C12(0.16667) C13(0.16667) C14(0.16667)
 C15(0.16667) C16(0.16667) C17(0.16667) C18(0.16667) C19(0.16667) C20(0.16667)
 C21(0.16667) C22(0.16667) C23(0.16667) C24(0.16667) C25(0.16667) C26(0.16667)
 C27(0.16667) C28(0.16667) C29(0.16667) C30(0.16667) C31(0.16667) C32(0.16667)
 C33(0.16667) C34(0.16667) C35(0.16667) C36(0.16667) C37(0.16667) C38(0.16667)
 C39(0.16667) C40(0.16667) C41(0.16667) C42(0.16667) C43(0.16667) C44(0.16667)
 C45(0.16667) C46(0.16667) C47(0.16667) C48(0.16667) C49(0.16667) C50(0.16667)
 C51(0.16667) C52(0.16667) C53(0.16667) C54(0.16667) C55(0.16667) C56(0.16667)
 C57(0.16667) C58(0.16667) C59(0.16667) C60(0.16667) C61(0.16667) C62(0.16667)
 C63(0.16667) C64(0.16667) C65(0.16667) C66(0.16667) C67(0.16667) C68(0.16667)
 C69(0.16667) C70(0.16667)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              67793
_shelx_hkl_checksum              43136
_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 1.196
_oxdiff_exptl_absorpt_empirical_full_min 0.839