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_4133375
_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            'C36 H508 Ce4 Mo132 N18 O629'
_chemical_formula_weight         24485.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   39.730(8)
_cell_length_b                   20.462(4)
_cell_length_c                   40.363(8)
_cell_measurement_reflns_used    75232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      1.09
_cell_volume                     32810(11)
_computing_cell_refinement
;
DIALS 2theta refinement, DIALS 1.6.2-g7df89bd4-release
;
_computing_data_collection       CrysAlisPro
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.6.2-g7df89bd4-release
pointless (Evans, P., 2006)
XIA2 0.5.328-gd3a94be2-dials-1.6-hotfix-5d8177 (Winter, G., 2010)
;
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            455608
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         0.497
_diffrn_source                   'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption 
correction using spherical harmonics
;
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             23316
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.187
_refine_diff_density_min         -1.510
_refine_diff_density_rms         0.335
_refine_ls_abs_structure_details
;
 Flack x determined using 51355 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6860
_refine_ls_number_reflns         139706
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+52.8427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2026
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                125240
_reflns_number_total             139706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3-rp366b2.cif
_cod_data_source_block           rp366b2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        32811(11)
_cod_original_sg_symbol_H-M      'P 2'
_cod_database_code               4133375
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.766
_shelx_estimated_absorpt_t_max   0.872
_shelx_res_checksum              45637
_shelx_hkl_checksum              80020