Synthesis, Characterization, and Theoretical Studies on Heterobinuclear (p-cymene)Os(μ-pz)2M (M = Ir, Rh; Hpz = Pyrazole) Complexes
Carmona, Daniel; Ferrer, Joaquina; Arilla, José M.; Reyes, Josefa; Lahoz, Fernando J.; Elipe, Sergio; Modrego, F. Javier; Oro, Luis A.; Organometallics 19 (2000) 798–; doi:10.1021/om990624h

data_4077662
_publ_section_title
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 Synthesis, Characterization, and Theoretical Studies on Heterobinuclear
 (p-cymene)Os(\m-pz)2M (M = Ir, Rh; Hpz = Pyrazole) Complexes
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_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              798
_journal_paper_doi               10.1021/om990624h
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C19 H20 N4 O3 Os Rh 1+, C24 H20 B 1-'
_chemical_formula_structural
'[(C10 H14) Os (C O) (C3 H3 N2)2 Rh (C O)2] [B (C6 H5)4]'
_chemical_formula_sum            'C43 H40 B N4 O3 Os Rh'
_chemical_formula_weight         964.71
_chemical_name_systematic
;
 tricarbonyl-(eta$6!-p-cymene)-bis-(mu!2$-pyrazolyl-N,N')-
 rhodium(i)-osmium(ii) tetraphenylborate
;
_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-97
_cell_angle_alpha                73.716(6)
_cell_angle_beta                 83.814(6)
_cell_angle_gamma                78.431(7)
_cell_formula_units_Z            2
_cell_length_a                   9.7378(8)
_cell_length_b                   11.2371(11)
_cell_length_c                   18.8008(14)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      10
_cell_volume                     1931.7(3)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP, SHELXTL v. 5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200.0(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9924
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.377
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details
;
 Azimuthal psi-scans of 12 reflections at 10\% intervals.
 Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.911
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=3D1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                6328
_reflns_number_total             8406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990624h.cif
_cod_data_source_block           compound8
_cod_depositor_comments
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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 
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_cod_database_code               4077662