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_4131595
_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
'C74.18 H133.09 Co12 N6.54 P8 Se16, Mo6 O19, 2(C4 H8 O)'
_chemical_formula_sum            'C82.18 H149.09 Co12 Mo6 N6.55 O21 P8 Se16'
_chemical_formula_weight         4358.84
_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             2017-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.65893(19)
_cell_length_b                   21.65893(19)
_cell_length_c                   28.9180(4)
_cell_measurement_reflns_used    16548
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1940
_cell_measurement_theta_min      3.0120
_cell_volume                     13565.7(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-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 0.993
_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    -66.00  30.00   1.00   15.00    --  -42.99  38.00  90.00   96
  2  \w   -116.00 -20.00   1.00   15.00    --  -42.99 -38.00  30.00   96
  3  \w     16.00 105.00   1.00   15.00    --   42.99  57.00 -90.00   89
  4  \w     87.00 158.00   1.00   60.00    --  111.00  61.00 120.00   71
  5  \w     72.00 133.00   1.00   60.00    --  111.00 -45.00 150.00   61
  6  \w     94.00 120.00   1.00   60.00    --  111.00  30.00-120.00   26
  7  \w     83.00 154.00   1.00   60.00    --  111.00  77.00-120.00   71
  8  \w    130.00 158.00   1.00   60.00    --  111.00  77.00 -90.00   28
  9  \w     81.00 109.00   1.00   60.00    --  111.00  77.00 -90.00   28
 10  \w     84.00 109.00   1.00   60.00    --  111.00  61.00 -30.00   25
 11  \w     97.00 158.00   1.00   60.00    --  111.00  30.00   0.00   61
 12  \w     59.00  98.00   1.00   60.00    --  111.00 -45.00  30.00   39
 13  \w    111.00 157.00   1.00   60.00    --  111.00  29.00  48.00   46
 14  \w     87.00 148.00   1.00   60.00    --  111.00  45.00-120.00   61
 15  \w     67.00 118.00   1.00   60.00    --  111.00 -30.00 -90.00   51
 16  \w    123.00 149.00   1.00   60.00    --  111.00  45.00 -90.00   26
 17  \w     80.00 154.00   1.00   60.00    --  111.00  77.00  60.00   74
;
_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      0.0151963000
_diffrn_orient_matrix_UB_12      0.0229499000
_diffrn_orient_matrix_UB_13      0.0491073000
_diffrn_orient_matrix_UB_21      -0.0666955000
_diffrn_orient_matrix_UB_22      -0.0140466000
_diffrn_orient_matrix_UB_23      0.0152727000
_diffrn_orient_matrix_UB_31      0.0195373000
_diffrn_orient_matrix_UB_32      -0.0658456000
_diffrn_orient_matrix_UB_33      0.0138661000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            77269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.753
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.774
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.134
_exptl_crystal_description       needle
_exptl_crystal_F_000             8384
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.251
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7126
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+21.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5917
_reflns_number_total             7126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07279_si_003.cif
_cod_data_source_block           protocloth
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4131595
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula
'c329.11 h573.67 n26.28 Co48 p32 Se64 Mo24 o84'
_reflns_odcompleteness_completeness 99.97
_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
 C36A-N39A
 1.33558 with sigma of 0.0001
 N39A-C40A
 1.14463 with sigma of 0.0001
 C36A-C40A
 2.48019 with sigma of 0.0001
 O41-C42 = O41-C45
 1.44 with sigma of 0.02
 C42-C43 = C43-C44 = C44-C45
 1.54 with sigma of 0.02
 C42-C45
 2.36 with sigma of 0.02
 O41-C43 = O41-C44 = C42-C44 = C43-C45
 2.38 with sigma of 0.02
 O41B-C42B = O41B-C45B
 1.44 with sigma of 0.02
 C42B-C43B = C43B-C44B = C44B-C45B
 1.54 with sigma of 0.02
 C42B-C45B
 2.36 with sigma of 0.02
 O41B-C43B = O41B-C44B = C42B-C44B = C43B-C45B
 2.38 with sigma of 0.02
 C42B-C12
 -3.8 with sigma of 0.02
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 0.01
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.04
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C31A, N32A, C33A, C34A, C35A, C36A, C37A, C38A, N39A, C40A, C31B, N32B, C33B,
 C34B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Co3, C31B, N32B, C33B, C34B, C35B} sigma for 1-2: 0.02, 1-3: 0.04
as
{Co3, C31A, N32A, C33A, C34A, C35A}
6. Others
 1*[1(DFIX)]+1*[1(DFIX)]-1*[1(DFIX)]=0 with esd of 0.0001
 Sof(C31B)=Sof(N32B)=Sof(C33B)=Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=1-FVAR(1)
 Sof(O41B)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=
 Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=0.5*(1-FVAR(2))
 Sof(O41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=0.5*FVAR(2)
 Sof(C31A)=Sof(N32A)=Sof(C33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(N39A)=Sof(C40A)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C21(H21A,H21B), C23(H23A,
 H23B), C25(H25A,H25B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,H44D), C45B(H45C,
 H45D)
7.b Aromatic/amide H refined with riding coordinates:
 C34A(H34A), C35A(H35A), C37A(H37A), C38A(H38A), C34B(H34B), C35B(H35B)
7.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.642