Transition metal incorporation into seleno-bridged cubane type clusters of molybdenum and tungsten. X-Ray crystal structures of the first [Mo3CuSe4] derivatives†
Llusar, Rosa; Uriel, Santiago; Vicent, Cristian; Journal of the Chemical Society, Dalton Transactions  (2001) 2813–; doi:10.1039/b104262a

data_7702638
_publ_section_title
;
 Transition metal incorporation into seleno-bridged cubane type clusters
 of molybdenum and tungsten. X-Ray crystal structures of the first
 [Mo3CuSe4] derivatives&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2813
_journal_paper_doi               10.1039/b104262a
_journal_year                    2001
_chemical_formula_sum            'C19 H48 Br4 Cl2 Cu F6 Mo3 P7 Se4'
_chemical_formula_weight         1665.10
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.7810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7990(5)
_cell_length_b                   23.8115(9)
_cell_length_c                   16.5128(6)
_cell_measurement_temperature    293(2)
_cell_volume                     5032.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31879
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    7.584
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.7115
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         10286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                6299
_reflns_number_total             10286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104262a.txt
_cod_data_source_block           '[Mo3CuSe4Br4(dmpe)3]PF6&#x00B7;CH2Cl2_(5)'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7702638