Steric Effects in the Oxidative Addition of MeI to a Sulfido-Bridged ZrRh2Early‒Late Heterobimetallic Compound
Nguyen, Duc Hanh; Modrego, F. Javier; Cetina-Casas, J. Miguel; Gómez-Bautista, Daniel; Jiménez, M. Victoria; Castarlenas, Ricardo; Lahoz, Fernando J.; Oro, Luis A.; Pérez-Torrente, Jesús J.; Organometallics 31 (2012) 6395–; doi:10.1021/om300629k

data_4079267
_publ_section_title
;
 Steric Effects in the Oxidative Addition of MeI to a Sulfido-Bridged
 ZrRh2Early--Late Heterobimetallic Compound
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6395
_journal_paper_doi               10.1021/om300629k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C45 H43 I O2 P2 Rh2 S2, 0.5 (C2 H4 Cl4)'
_chemical_formula_sum            'C46 H45 Cl2 I O2 P2 Rh2 S2'
_chemical_formula_weight         1159.50
_chemical_name_systematic
; 
 ? 
;
_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                94.0330(10)
_cell_angle_beta                 90.0520(10)
_cell_angle_gamma                100.0170(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8840(6)
_cell_length_b                   12.5542(7)
_cell_length_c                   18.2476(10)
_cell_measurement_reflns_used    5383
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.24
_cell_volume                     2224.0(2)
_computing_cell_refinement       'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.45 (Bruker AXS, 2003)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22065
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.8677
_exptl_absorpt_correction_T_min  0.7600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.45.                    
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10383
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0429P)^2^+1.4504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                8586
_reflns_number_total             10383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300629k_si_002.cif
_cod_data_source_block           compnd_5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4079267