Weaving Nanoscale Cloth through Electrostatic Templating.
Champsaur, Anouck M.; Mézière, Cécile; Allain, Magali; Paley, Daniel W.; Steigerwald, Michael L.; Nuckolls, Colin; Batail, Patrick; Journal of the American Chemical Society 139 (2017) 11718–11721; doi:10.1021/jacs.7b07279

data_4131594
_publ_section_title
;
 Weaving Nanoscale Cloth through Electrostatic Templating.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11718
_journal_page_last               11721
_journal_paper_doi               10.1021/jacs.7b07279
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '2(C32 H64 Co6 N2 P4 Se8), Mo6 O19'
_chemical_formula_sum            'C64 H128 Co12 Mo6 N4 O19 P8 Se16'
_chemical_formula_weight         4051.62
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4506(17)
_cell_length_b                   21.4506(17)
_cell_length_c                   28.554(3)
_cell_measurement_reflns_used    860
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      71.2380
_cell_measurement_theta_min      4.1050
_cell_volume                     13139(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -79.00 -43.00   1.00   50.00    --  -42.99 -38.00 -60.00   36
  2  \w    -28.00  62.00   1.00   50.00    --   42.99 -38.00  90.00   90
  3  \w    101.00 157.00   1.00  220.00    --  111.00  77.00-150.00   56
  4  \w     87.00 112.00   1.00  220.00    --  111.00  45.00 -60.00   25
  5  \w     87.00 119.00   1.00  220.00    --  111.00  45.00-150.00   32
  6  \w    112.00 158.00   1.00  220.00    --  111.00  61.00  60.00   46
  7  \w     84.00 109.00   1.00  220.00    --  111.00  61.00 -60.00   25
  8  \w     87.00 154.00   1.00  220.00    --  111.00  30.00   0.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0119662000
_diffrn_orient_matrix_UB_12      0.0598649000
_diffrn_orient_matrix_UB_13      -0.0284976000
_diffrn_orient_matrix_UB_21      0.0528784000
_diffrn_orient_matrix_UB_22      0.0181400000
_diffrn_orient_matrix_UB_23      0.0338783000
_diffrn_orient_matrix_UB_31      0.0471113000
_diffrn_orient_matrix_UB_32      -0.0353658000
_diffrn_orient_matrix_UB_33      -0.0307901000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2232
_diffrn_reflns_av_unetI/netI     0.1635
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24230
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        65.077
_diffrn_reflns_theta_max         65.077
_diffrn_reflns_theta_min         2.913
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.400
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    2.048
_exptl_crystal_description       needle
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1906
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1003P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.3005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2438
_reflns_number_total             5612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07279_si_002.cif
_cod_data_source_block           cloth
_cod_original_cell_volume        13138(3)
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4131594
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C64 H126 Co12 Mo6 N4 O19 P8 Se16'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33B-C34B_$2 = C33B-C35B_$2
 3.5 with sigma of 0.02
 C33B-C35B = C33B-C34B_$1
 2.46 with sigma of 0.02
 C34B-C35B_$1
 2.48 with sigma of 0.02
 C35B-C33B_$1
 1.42 with sigma of 0.02
3. Restrained planarity
 C33B, C34B, C35B, C33B_$1, C34B_$1, C35B_$1, N32B, N32B_$1
 with sigma of 0.2
4. 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 0.01 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 Se1B, Se2B, Se3B, Se4B, Co1B, P11B, C12B, C13B, C14B, C15B, C16B, C17B, Co2B,
 P21B, C22B, C23B, C24B, C25B, C26B, C27B, Co3B, C31B, N32B, C33B, C34B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{Se1B, Se2B, Se3B, Se4B, Co1B, P11B, C12B, C13B, C14B, C15B, C16B, C17B, Co2B,
P21B, C22B, C23B, C24B, C25B, C26B, C27B, Co3B, C31B, N32B, C33B, C34B, C35B}
sigma for 1-2: 0.005, 1-3: 0.005
as
{Se1, Se2, Se3, Se4, Co1, P11, C12, C13, C14, C15, C16, C17, Co2, P21, C22,
C23, C24, C25, C26, C27, Co3, C31, N32, C33, C34, C35}
7. Others
 Sof(Se1B)=Sof(Se2B)=Sof(Se3B)=Sof(Se4B)=Sof(Co1B)=Sof(P11B)=Sof(C12B)=
 Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=
 Sof(H14C)=Sof(H14D)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(Co2B)=
 Sof(P21B)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(Co3B)=Sof(C31B)=Sof(N32B)=Sof(C33B)=Sof(C34B)=Sof(H34B)=
 Sof(C35B)=Sof(H35B)=1-FVAR(1)
 Sof(Se1)=Sof(Se2)=Sof(Se3)=Sof(Se4)=Sof(Co1)=Sof(P11)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(Co2)=Sof(P21)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=Sof(Co3)=Sof(C31)=Sof(N32)=Sof(C33)=Sof(C34)=Sof(H34)=
 Sof(C35)=Sof(H35)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C22(H22A,H22B), C24(H24A,
 H24B), C26(H26A,H26B), C12B(H12C,H12D), C14B(H14C,H14D), C16B(H16C,H16D),
 C22B(H22C,H22D), C24B(H24C,H24D), C26B(H26C,H26D)
8.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C13B(H13D,H13E,H13F),
 C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F), C23B(H23D,H23E,H23F), C25B(H25D,
 H25E,H25F), C27B(H27D,H27E,H27F)
8.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C34B(H34B), C35B(H35B)
;
_shelx_res_checksum              84254
_shelx_hkl_checksum              61886
_shelx_fab_checksum              9794
_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 2.000
_oxdiff_exptl_absorpt_empirical_full_min 0.297