Mono- and Bis(hydrazine) Complexes of Osmium(II): Synthesis, Reactions, and X-ray Crystal Structure of the [Os(NH2NH2)2{P(OEt)3}4](BPh4)2 Derivative
Gabriele Albertin; Stefano Antoniutti; Alessia Bacchi; Massimo Bergamo; Emilio Bordignon; Giancarlo Pelizzi; Inorganic Chemistry 37 (1998) 479–489; doi:10.1021/ic970463e

data_4322629
_publ_section_title
;
 Mono- and Bis(hydrazine) Complexes of Osmium(II): Synthesis, Reactions,
 and X-ray Crystal Structure of the [Os(NH2NH2)2{P(OEt)3}4](BPh4)2
 Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              479
_journal_page_last               489
_journal_paper_doi               10.1021/ic970463e
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C74 H114 B2 N4 O13 Os P4'
_chemical_formula_weight         1603.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.84(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.550(4)
_cell_length_b                   19.663(4)
_cell_length_c                   20.843(4)
_cell_measurement_temperature    293(2)
_cell_volume                     8298(4)
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 diffractometer'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1307
_diffrn_reflns_av_sigmaI/netI    0.3417
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16177
_diffrn_reflns_theta_max         70.35
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        52
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    4.096
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             3344
_refine_diff_density_max         0.548
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.842
_refine_ls_goodness_of_fit_obs   1.167
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         15738
_refine_ls_number_restraints     927
_refine_ls_restrained_S_all      0.824
_refine_ls_restrained_S_obs      1.023
_refine_ls_R_factor_all          0.3598
_refine_ls_R_factor_obs          0.0909
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3906
_refine_ls_wR_factor_obs         0.2168
_reflns_number_observed          2967
_reflns_number_total             15738
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970463e.cif
_cod_data_source_block
Compound_[Os(NH2NH2)2{P(OEt)3}4](BPh4)2.C2H5OH-4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1700P)^2^+0.0000P] 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^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8298(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4322629