Unusual Ligand Transformations Initiated by dppm Deprotonation in Methylene-Bridged Rh/Os Complexes
Kyle D. Wells; Robert McDonald; Michael J. Ferguson; Martin Cowie; Inorganic Chemistry 50 (2011) 3523–3538; doi:10.1021/ic102470j

data_4324875
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       martin.cowie@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr. Martin Cowie'
_publ_contact_author_phone       1(780)4925581
_publ_section_title
;
 Unusual Ligand Transformations Initiated by dppm Deprotonation in
 Methylene-Bridged Rh/Os Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3523
_journal_page_last               3538
_journal_paper_doi               10.1021/ic102470j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C59 H57 O3 Os P4 Rh'
_chemical_formula_weight         1231.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.890(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.276(2)
_cell_length_b                   18.850(3)
_cell_length_c                   18.317(2)
_cell_measurement_reflns_used    6841
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.10
_cell_volume                     5262.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44909
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    2.892
_exptl_absorpt_correction_T_max  0.4198
_exptl_absorpt_correction_T_min  0.2815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.622
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         12079
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+4.8221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                10669
_reflns_number_total             12079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102470j_si_002_2.cif
_cod_data_source_block           5
_cod_original_cell_volume        5262.4(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324875