Reversible Opening of the Triangular Structure of a Sulfido-Bridged ZrRh2Early−Late Heterobimetallic Complex Induced by Bis-(diphenylphosphino)methane
Hernandez-Gruel, Marc A. F.; Lahoz, Fernando J.; Dobrinovich, Isabel T.; Modrego, F. Javier; Oro, Luis A.; Pérez-Torrente, Jesús J.; Organometallics 26 (2007) 2616–; doi:10.1021/om061092p

data_4072855
_publ_section_title
;
 Reversible Opening of the Triangular Structure of a Sulfido-Bridged
 ZrRh2Early&#x2212;Late Heterobimetallic Complex Induced by
 Bis-(diphenylphosphino)methane
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2616
_journal_paper_doi               10.1021/om061092p
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C78 H86 O2 P4 Rh2 S2 Zr, 2.5 (C7 H8)'
_chemical_formula_sum            'C95.5 H106 O2 P4 Rh2 S2 Zr'
_chemical_formula_weight         1770.84
_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                97.010(2)
_cell_angle_beta                 99.872(2)
_cell_angle_gamma                101.853(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5217(13)
_cell_length_b                   14.9233(14)
_cell_length_c                   23.258(2)
_cell_measurement_reflns_used    2893
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      2.31
_cell_volume                     4464.5(7)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_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      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26189
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS
    within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1834
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.135
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         17167
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1882
_reflns_number_gt                10809
_reflns_number_total             17167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061092psi20061206_020733.cif
_cod_data_source_block           compdound_3
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C95.50 H106 O2 P4 Rh2 S2 Zr'
_cod_database_code               4072855