Homo- and hetero-metallic rhenium oxomethoxide complexes with a M4(µ-O)2(µ-OMe)4 planar core—a new family of metal alkoxides displaying a peculiar structural disorder. Preparation and X-ray single crystal study
Seisenbaeva, Gulaim A.; Shevelkov, Andrei V.; Tegenfeldt, Jörgen; Kloo, Lars; Drobot, Dmitrii V.; Kessler, Vadim G.; Journal of the Chemical Society, Dalton Transactions  (2001) 2762–; doi:10.1039/b103287a

data_7702604
_publ_section_title
;
 Homo- and hetero-metallic rhenium oxomethoxide complexes with a
 M4(&#x00B5;-O)2(&#x00B5;-OMe)4 planar core---a new family of metal
 alkoxides displaying a peculiar structural disorder. Preparation and
 X-ray single crystal study
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2762
_journal_paper_doi               10.1039/b103287a
_journal_year                    2001
_chemical_formula_sum            'C12 H36 Mo2.4 O18 Re1.6'
_chemical_formula_weight         996.57
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.41(2)
_cell_angle_beta                 92.92(2)
_cell_angle_gamma                92.71(3)
_cell_formula_units_Z            3
_cell_length_a                   7.905(2)
_cell_length_b                   15.997(4)
_cell_length_c                   17.519(6)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.39
_cell_volume                     2024.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.858
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       'SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.1169
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11977
_diffrn_reflns_theta_full        28.40
_diffrn_reflns_theta_max         28.40
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.3110
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'reddish black'
_exptl_crystal_density_diffrn    2.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             473
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.331
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       0.00060(6)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8733
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.191
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                5036
_reflns_number_total             8733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103287a.txt
_cod_data_source_block           moreme11
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' 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.

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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_cell_volume        2024.9(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702604