Stereoselective Assembly of Gigantic Chiral Molybdenum Blue Wheels Using Lanthanide Ions and Amino Acids.
Xuan, Weimin; Pow, Robert; Watfa, Nancy; Zheng, Qi; Surman, Andrew J.; Long, De-Liang; Cronin, Leroy; Journal of the American Chemical Society 141 (2019) 1242–1250; doi:10.1021/jacs.8b09750

data_4133369
_publ_section_title
;
 Stereoselective Assembly of Gigantic Chiral Molybdenum Blue Wheels Using
 Lanthanide Ions and Amino Acids.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1242
_journal_page_last               1250
_journal_paper_doi               10.1021/jacs.8b09750
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration none
_chemical_formula_sum            'C86 H534 Ce4 Mo124 N16 Na2 O604'
_chemical_formula_weight         23962.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.9681(11)
_cell_length_b                   45.6548(15)
_cell_length_c                   20.6531(7)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.20
_cell_volume                     32971.9(19)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            432791
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         0.986
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    2.656
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5797
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    2.414
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             22912
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.879
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Flack x determined using 27787 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3455
_refine_ls_number_reflns         64775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+367.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                61336
_reflns_number_total             64775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4-d-wx7683.cif
_cod_data_source_block           wx7683
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct methods' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4133369
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              52678
_shelx_hkl_checksum              5267