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_7057524
_publ_section_title
;
 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
'2(C78 H72 Br3.81 Ga0.81 P6 S4 W3), 10(C4 H8 O)'
_chemical_formula_sum            'C196 H224 Br7.63 Ga1.63 O10 P12 S8 W6'
_chemical_formula_weight         5193.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.5160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.4088(13)
_cell_length_b                   18.0186(6)
_cell_length_c                   28.4195(9)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.45
_cell_volume                     19859.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXT (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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55752
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.522
_exptl_absorpt_coefficient_mu    5.447
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.1706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0921 before and 0.0509 after correction. The Ratio of minimum to maximum transmission is 0.6556. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             10038
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.093
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         17525
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+220.8660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13983
_reflns_number_total             17525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00650d2.cif
_cod_data_source_block           pe_569
_cod_depositor_comments
'Adding full bibliography for 7057524--7057525.cif.'
_cod_database_code               7057524
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.252
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O31S-C32S = C32S-C33S = C33S-C34S = C35S-C34S = O31S-C35S
 1.45 with sigma of 0.02
 O41S-C42S = C42S-C43S = C43S-C44S = C45S-C44S = O41S-C45S
 1.45 with sigma of 0.02
 C52S-C53S = C52S-O51S = O51S-C55S = C54S-C55S = C54S-C53S
 1.45 with sigma of 0.02
 C33S-O31S
 2.35 with sigma of 0.04
 C33S-C35S
 2.35 with sigma of 0.04
 C32S-C34S
 2.35 with sigma of 0.04
 C32S-C35S
 2.35 with sigma of 0.04
 C35S-C33S
 2.35 with sigma of 0.04
 C43S-O41S
 2.35 with sigma of 0.04
 C43S-C45S
 2.35 with sigma of 0.04
 C42S-C44S
 2.35 with sigma of 0.04
 C42S-C45S
 2.35 with sigma of 0.04
 C45S-C43S
 2.35 with sigma of 0.04
 C52S-C55S
 2.35 with sigma of 0.04
 C52S-C54S
 2.35 with sigma of 0.04
 O51S-C53S
 2.35 with sigma of 0.04
 O51S-C54S
 2.35 with sigma of 0.04
 C53S-C55S
 2.35 with sigma of 0.04
3. Others
 Sof(Br4)=Sof(Ga1)=FVAR(1)
 Fixed Sof: C55S(0.5) H55A(0.5) H55B(0.5) O51S(0.5) C52S(0.5) H52A(0.5)
 H52B(0.5) C53S(0.5) H53A(0.5) H53B(0.5) C54S(0.5) H54A(0.5) H54B(0.5)
4.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), C22S(H22C,H22D), C24S(H24A,H24B), C25S(H25A,H25B),
 C23S(H23A,H23B), C15S(H15A,H15B), C32S(H32C,H32D), C33S(H33A,H33B), C35S(H35A,
 H35B), C12S(H12C,H12D), C34S(H34A,H34B), C13S(H13A,H13B), C14S(H14A,H14B),
 C55S(H55A,H55B), C52S(H52A,H52B), C53S(H53A,H53B), C54S(H54A,H54B), C42S(H42A,
 H42B), C43S(H43A,H43B), C45S(H45A,H45B), C44S(H44A,H44B)
4.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)
;
_smtbx_masks_special_details
;
Some of the solvent tetrahydrofuran molecules appeared to be highly disordered
and it was difficult to model their positions reliably. Therefore, the structure 
was treated via Solvent Mask procedure to remove the contribution
of the electron density in the solvent regions from the intensity data.
The total potential solvent accessible void volume was estimated to be
ca.  650 Ang**3 and the electron count per unit cell was 280, which
were assigned to 4 THF molecules per unit cell and one THF
molecule per formula unit.
;
_shelx_res_checksum              97231
_shelx_fab_checksum              46334
_olex2_submission_special_instructions 'No special instructions were received'