Carbidoheptarhenate Complexes of Mercury Hydroxide and Arenethiolate. Crystal Structures of [NEt3Bz]2[Re7C(CO)21HgOH] and [PPh4]2[Re7C(CO)21HgSC6H4Br]
Udo Brand; Jeffery L. Coffer; Timothy J. Henly; Scott R. Wilson; John R. Shapley; Inorganic Chemistry 36 (1997) 3386–3389; doi:10.1021/ic970068o

data_4323506
_publ_section_title
;
 Carbidoheptarhenate Complexes of Mercury Hydroxide and Arenethiolate.
 Crystal Structures of [NEt3Bz]2[Re7C(CO)21HgOH] and
 [PPh4]2[Re7C(CO)21HgSC6H4Br]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3386
_journal_page_last               3389
_journal_paper_doi               10.1021/ic970068o
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C76.5 H45 Br Cl Hg O21 P2 Re7 S'
_chemical_formula_weight         3013.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                79.3900(10)
_cell_angle_beta                 79.9270(10)
_cell_angle_gamma                65.5110(10)
_cell_formula_units_Z            2
_cell_length_a                   12.40990(10)
_cell_length_b                   13.76390(10)
_cell_length_c                   25.8584(5)
_cell_measurement_temperature    198(2)
_cell_volume                     3926.72(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15202
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    13.371
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.549
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platy
_exptl_crystal_F_000             2750
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         7915
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.136
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_obs          0.0433
_refine_ls_shift/esd_max         0.105
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+19.3680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1021
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          5713
_reflns_number_total             8970
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970068o.cif
_cod_data_source_block           u3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+19.3680P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+19.3680P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C76.50 H45 Br Cl Hg O21 P2 Re7 S'
_cod_database_code               4323506