The first heterocubane cluster with a [W3GaS4] core
Petrov, Pavel A.; Nadolinny, Vladimir A.; Bogomyakov, Artem S.; Sukhikh, Taisiya S.; New Journal of Chemistry 42 (2018) 12349–; doi:10.1039/C8NJ00650D

data_7057525
_publ_section_title
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 The first heterocubane cluster with a [W3GaS4] core
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12349
_journal_paper_doi               10.1039/C8NJ00650D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C78 H72 Cl4 Ga Mo3 P6 S4, 3(C4 H8 O)'
_chemical_formula_sum            'C90 H96 Cl4 Ga Mo3 O3 P6 S4'
_chemical_formula_weight         2039.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-12-26 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6347(5)
_cell_length_b                   21.1225(5)
_cell_length_c                   21.2228(5)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.37
_cell_volume                     8800.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.360
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0489 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.8624. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             4156
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         17994
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0390P)^2^+18.2960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15370
_reflns_number_total             17994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00650d2.cif
_cod_data_source_block           pe_448_3
_cod_depositor_comments
'Adding full bibliography for 7057524--7057525.cif.'
_cod_database_code               7057525
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.656
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C44S-C45S
 1.45 with sigma of 0.01
 C42S-C43S
 1.45 with sigma of 0.01
 C44S-C43S
 1.45 with sigma of 0.01
 C42S-O41S
 1.45 with sigma of 0.01
 C45S-O41S
 1.45 with sigma of 0.01
 O31S-C35S = O31S-C32S = C35S-C34S = C34S-C33S = C33S-C32S
 1.45 with sigma of 0.01
 C25S-C24S
 1.45 with sigma of 0.02
 C22S-C23S
 1.45 with sigma of 0.02
 C24S-C23S
 1.45 with sigma of 0.02
 C25S-O21S
 1.45 with sigma of 0.02
 C22S-O21S
 1.45 with sigma of 0.02
 O51S-C52S = C53S-C52S = C54S-C53S = C55S-C54S = O51S-C55S
 1.45 with sigma of 0.01
 O41S-C43S
 2.35 with sigma of 0.02
 O41S-C44S
 2.35 with sigma of 0.02
 C43S-C45S
 2.35 with sigma of 0.02
 C45S-C42S
 2.35 with sigma of 0.02
 C44S-C42S
 2.35 with sigma of 0.02
 O31S-C34S
 2.35 with sigma of 0.02
 O31S-C33S
 2.35 with sigma of 0.02
 C35S-C32S
 2.35 with sigma of 0.02
 C35S-C33S
 2.35 with sigma of 0.02
 C32S-C34S
 2.35 with sigma of 0.02
 O51S-C53S
 2.35 with sigma of 0.02
 O51S-C54S
 2.35 with sigma of 0.02
 C52S-C55S
 2.35 with sigma of 0.02
 C55S-C53S
 2.35 with sigma of 0.02
 C52S-C54S
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O41S) = Uiso(C42S) = Uiso(C43S) = Uiso(C44S) = Uiso(C45S) = Uiso(O51S) =
Uiso(C52S) = Uiso(C53S) = Uiso(C54S) = Uiso(C55S)
Uiso(C22S) = Uiso(O21S) = Uiso(C25S) = Uiso(C23S) = Uiso(C24S) = Uiso(O31S) =
Uiso(C32S) = Uiso(C33S) = Uiso(C35S) = Uiso(C34S)
4. Others
 Sof(O51S)=Sof(C52S)=Sof(H52A)=Sof(H52B)=Sof(C53S)=Sof(H53B)=Sof(H53A)=
 Sof(C54S)=Sof(H54A)=Sof(H54B)=Sof(C55S)=Sof(H55A)=Sof(H55B)=1-FVAR(1)
 Sof(O41S)=Sof(C44S)=Sof(H44A)=Sof(H44B)=Sof(C42S)=Sof(H42A)=Sof(H42B)=
 Sof(C43S)=Sof(H43A)=Sof(H43B)=Sof(C45S)=Sof(H45A)=Sof(H45B)=FVAR(1)
 Sof(O31S)=Sof(C35S)=Sof(H35A)=Sof(H35B)=Sof(C33S)=Sof(H33A)=Sof(H33B)=
 Sof(C34S)=Sof(H34A)=Sof(H34B)=Sof(C32S)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(O21S)=Sof(C22S)=Sof(H22C)=Sof(H22D)=Sof(C23S)=Sof(H23A)=Sof(H23B)=
 Sof(C24S)=Sof(H24A)=Sof(H24B)=Sof(C25S)=Sof(H25A)=Sof(H25B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C21(H21A,H21B), C22(H22A,H22B), C31(H31A,
 H31B), C32(H32A,H32B), C52S(H52A,H52B), C53S(H53B,H53A), C54S(H54A,H54B),
 C55S(H55A,H55B), C12S(H12C,H12D), C13S(H13A,H13B), C14S(H14A,H14B), C15S(H15A,
 H15B), C22S(H22C,H22D), C23S(H23A,H23B), C24S(H24A,H24B), C25S(H25A,H25B),
 C44S(H44A,H44B), C42S(H42A,H42B), C35S(H35A,H35B), C33S(H33A,H33B), C43S(H43A,
 H43B), C34S(H34A,H34B), C32S(H32C,H32D), C45S(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C142(H142), C143(H143), C144(H144),
 C145(H145), C146(H146), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C222(H222), C223(H223), C224(H224), C225(H225), C226(H226),
 C232(H232), C233(H233), C234(H234), C235(H235), C236(H236), C242(H242),
 C243(H243), C244(H244), C245(H245), C246(H246), C312(H312), C313(H313),
 C314(H314), C315(H315), C316(H316), C322(H322), C323(H323), C324(H324),
 C325(H325), C326(H326), C332(H332), C333(H333), C334(H334), C335(H335),
 C336(H336), C342(H342), C343(H343), C344(H344), C345(H345), C346(H346)
;
_olex2_submission_special_instructions 'No special instructions were received'