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_7038997
_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, 3(C7 H8), B1 F4'
_chemical_formula_sum            'C72 H84 B Cl3 F4 Mo3 N3 P3 S4'
_chemical_formula_weight         1693.55
_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                   19.5506(3)
_cell_length_b                   19.5506(3)
_cell_length_c                   19.5506(3)
_cell_measurement_reflns_used    11928
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      28.6730
_cell_measurement_theta_min      3.7580
_cell_volume                     7472.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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(14)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega   44.00  107.20   0.8000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  178.0000  -30.0000 79

  2 omega  -10.00   24.40   0.8000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814   38.0000   30.0000 43

  3 omega  -63.00    3.40   0.8000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       14.6814  -57.0000   30.0000 83
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0167313000
_diffrn_orient_matrix_UB_12      -0.0038858000
_diffrn_orient_matrix_UB_13      -0.0319648000
_diffrn_orient_matrix_UB_21      -0.0227694000
_diffrn_orient_matrix_UB_22      -0.0268418000
_diffrn_orient_matrix_UB_23      -0.0086640000
_diffrn_orient_matrix_UB_31      -0.0227391000
_diffrn_orient_matrix_UB_32      0.0241002000
_diffrn_orient_matrix_UB_33      -0.0148365000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.325
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.505
_exptl_crystal_description       prism
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.2206
_exptl_crystal_size_mid          0.1854
_exptl_crystal_size_min          0.1613
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 2230 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+17.1998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                5337
_reflns_number_total             6384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00755d2.cif
_cod_data_source_block           exp_2437
_cod_depositor_comments
'Adding full bibliography for 7038996--7038997.cif.'
_cod_original_cell_volume        7472.7(3)
_cod_database_code               7038997
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C51 H60 B F4 N2 P3 S4 Mo3'
_reflns_odcompleteness_completeness 99.75
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B), C15(H15A,H15B), C2AA(H2AA,H2AB)
2.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA), C5(H5), C5AA(H5AA), C9(H9), C12(H12), C16(H16),
 C17(H17), C3AA(H3AA), C4AA(H4AA), C4(H4), C6AA(H6AA), C6(H6), C8(H8), C10(H10)
2.d Idealised Me refined as rotating group:
 C7AA(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              46663
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2014-01-15
_olex2_submission_special_instructions 'No special instructions were received'