Crystal structure of [[Mo3Se7(S2CNEt2)3]2(μ-Se)] ⋅ 2(C6H4Cl2), C42H68Cl4Mo6N6S12Se15
Brakefield, Kyra; Barnes, Justin; Donahue, James P.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 739–743; doi:10.1515/ncrs-2019-0938

data_8105274
_publ_section_title
;
 Crystal structure of [[Mo3Se7(S2CNEt2)3]2(\m-Se)] &#x22C5; 2(C6H4Cl2),
 C42H68Cl4Mo6N6S12Se15
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              739
_journal_page_last               743
_journal_paper_doi               10.1515/ncrs-2019-0938
_journal_volume                  235
_journal_year                    2020
_chemical_formula_sum            'C42 H68 Cl4 Mo6 N6 S12 Se15'
_chemical_formula_weight         2943.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                117.446(2)
_cell_angle_beta                 99.775(2)
_cell_angle_gamma                98.233(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0196(19)
_cell_length_b                   18.813(3)
_cell_length_c                   19.745(3)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.7595
_cell_measurement_theta_min      2.188
_cell_volume                     4091.8(11)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2016)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Bruker, 2016)'
_computing_publication_material  '<i>SHELXTL</i> (Bruker, 2016)'
_computing_structure_refinement  '<i>SHELXL-2018/1</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXT 2014/5</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0492
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18161
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        18.759
_diffrn_reflns_theta_max         18.759
_diffrn_reflns_theta_min         1.641
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.035
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.4498
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.220
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         6294
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0557
_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^)+(0.1128P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4913
_reflns_number_total             6294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0938_suppl.cif
_cod_data_source_block           JPD981_0m_a
_cod_original_cell_volume        4091.7(10)
_cod_database_code               8105274
_shelx_estimated_absorpt_t_min   0.214
_shelx_estimated_absorpt_t_max   0.680
_exptl_absorpt_special_details   '<i>SADABS</i> (Krause <i>et al.</i>, 2015)'