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_4077664
_publ_section_title
;
 Synthesis, Characterization, and Theoretical Studies on Heterobinuclear
 (p-cymene)Os(\m-pz)2M (M = Ir, Rh; Hpz = Pyrazole) Complexes
;
_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         'C17 H20 I N4 O Os Rh'
_chemical_formula_structural     '[(C10 H14) Os (C3 H3 N2)2 Rh I (C O)]'
_chemical_formula_sum            'C17 H20 I N4 O Os Rh'
_chemical_formula_weight         716.38
_chemical_name_systematic
;
 iodo-carbonyl-(eta$6!-p-cymene)-bis-(mu!2$-pyrazolyl-N,N')-
 rhodium(i)-osmium(ii)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.544(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2213(15)
_cell_length_b                   13.577(2)
_cell_length_c                   16.009(2)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      12.7
_cell_volume                     1956.4(5)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_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  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5803
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.922
_exptl_absorpt_correction_T_max  0.062
_exptl_absorpt_correction_T_min  0.035
_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    2.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0425
_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=3D1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                2381
_reflns_number_total             3438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990624h.cif
_cod_data_source_block           compound12
_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 
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_cod_original_cell_volume        1956.5(5)
_cod_database_code               4077664