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_4077663
_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         'C18 H20 I Ir N4 O2 Os'
_chemical_formula_structural     '[(C10 H14) Os (C3 H3 N2)2 Rh I (C O)2]'
_chemical_formula_sum            'C18 H20 I Ir N4 O2 Os'
_chemical_formula_weight         833.68
_chemical_name_systematic
;
 iodo-dicarbonyl-(eta$6!-p-cymene)-bis-(mu!2$-pyrazolyl-N,N')-
 iridium(i)-osmium(ii)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5321(11)
_cell_length_b                   12.7061(15)
_cell_length_c                   17.9660(13)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      19.1
_cell_measurement_theta_min      12.85
_cell_volume                     2176.0(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4755
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.381
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
 Data corrected with the program DIFABS.
 The correction carried out by this program is based on the following
 correction factors: max. absorption correction factor 1.271, and
 min. absorption correction factor 0.751.
 (N. Walker, D. Stuart, Acta Crystallogr., Sect. A, 39, 158 (1983))
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0160P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                3263
_reflns_number_total             3832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990624h.cif
_cod_data_source_block           compound10
_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_database_code               4077663