Synthesis and Characterization of Osmium(II) Trispyrazolylborate Complexes
Dickinson, Paul W.; Girolami, Gregory S.; Inorganic Chemistry 45 (2006) 5215–5224; doi:10.1021/ic0602291

data_4332310
_publ_contact_author             'Gregory S. Girolami'
_publ_section_title
;
 Synthesis and Characterization of Osmium(II) Trispyrazolylborate
 Complexes
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5215
_journal_page_last               5224
_journal_paper_doi               10.1021/ic0602291
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C18 H25 B N6 O Os, C H4 O'
_chemical_formula_sum            'C19 H29 B N6 O2 Os'
_chemical_formula_weight         574.49
_chemical_melting_point          198
_chemical_name_common            TpOs(cod)OMe*MeOH
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 102.418(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7281(14)
_cell_length_b                   14.0044(19)
_cell_length_c                   13.9058(18)
_cell_measurement_reflns_used    19322
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.09
_cell_volume                     2040.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19322
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.279
_exptl_absorpt_correction_T_max  0.6981
_exptl_absorpt_correction_T_min  0.3468
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.890
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                4082
_reflns_number_total             5004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0602291sup1.cif
_cod_data_source_block           f17afa14
_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 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4332310