C3-symmetry Mo3S4 aminophosphino clusters combining three sources of stereogenicity: stereocontrol directed by hydrogen bond interactions and ligand configuration.
Alfonso, Carmina; Feliz, Marta; Safont, Vicent S.; Llusar, Rosa; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7829–7835; doi:10.1039/c6dt00755d

data_7038996
_publ_section_title
;
 C3-symmetry Mo3S4 aminophosphino clusters combining three sources of
 stereogenicity: stereocontrol directed by hydrogen bond interactions and
 ligand configuration.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7829
_journal_page_last               7835
_journal_paper_doi               10.1039/c6dt00755d
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C51 H60 Cl3 Mo3 N3 P3 S4, B1 F4'
_chemical_formula_sum            'C51 H60 B Cl3 F4 Mo3 N3 P3 S4'
_chemical_formula_weight         1417.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-15 deposited with the CCDC.
2016-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0728(2)
_cell_length_b                   19.0728(2)
_cell_length_c                   19.0728(2)
_cell_measurement_reflns_used    6850
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.3790
_cell_measurement_theta_min      3.8290
_cell_volume                     6938.14(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -97.00  -34.00   1.0000  116.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.6603  -57.0000    0.0000 63

  2 omega  -67.00  -32.00   1.0000  116.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9103  -51.0000   48.0000 35
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0024847000
_diffrn_orient_matrix_UB_12      0.0152801000
_diffrn_orient_matrix_UB_13      0.0337726000
_diffrn_orient_matrix_UB_21      0.0124442000
_diffrn_orient_matrix_UB_22      -0.0316281000
_diffrn_orient_matrix_UB_23      0.0152121000
_diffrn_orient_matrix_UB_31      0.0349723000
_diffrn_orient_matrix_UB_32      0.0122630000
_diffrn_orient_matrix_UB_33      -0.0029715000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14383
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.1421
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.0933
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 1526 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+5.9961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1535
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.910
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                3632
_reflns_number_total             3964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00755d2.cif
_cod_data_source_block           str1507
_cod_depositor_comments
'Adding full bibliography for 7038996--7038997.cif.'
_cod_original_cell_volume        6938.1(2)
_cod_database_code               7038996
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C51 H60 F6 N3 P4 Cl3 S4 Mo3'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C1(H1A,H1B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C14(H14), C9(H9), C15(H15), C17(H17), C11(H11), C16(H16),
 C10(H10), C8(H8)
;
_shelx_res_checksum              12472
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2013-05-16
_olex2_submission_special_instructions 'No special instructions were received'