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_7702637
_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            'C18 H48 Cl4 Cu F6 Mo3 P7 Se4'
_chemical_formula_weight         1404.35
_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                 90.180(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.607(6)
_cell_length_b                   15.879(8)
_cell_length_c                   21.314(11)
_cell_measurement_temperature    293(2)
_cell_volume                     4267(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1368
_diffrn_reflns_av_sigmaI/netI    0.2202
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18013
_diffrn_reflns_theta_full        22.01
_diffrn_reflns_theta_max         22.01
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    5.320
_exptl_absorpt_correction_T_max  1.955437
_exptl_absorpt_correction_T_min  1.349658
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.883
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                2474
_reflns_number_total             5215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104262a.txt
_cod_data_source_block           '[Mo3CuSe4Cl4(dmpe)4]PF6_(4)'
_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               7702637