Ligand Effects on the Oxidative Addition of Halogens to (dpp-nacnacR)Rh(phdi)
David W. Shaffer; Scott A. Ryken; Ryan A. Zarkesh; Alan F. Heyduk; Inorganic Chemistry 51 (2012) 12122–12131; doi:10.1021/ic300733j

data_4330990
_publ_section_title
;
 Ligand Effects on the Oxidative Addition of Halogens to
 (dpp-nacnacR)Rh(phdi)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12122
_journal_page_last               12131
_journal_paper_doi               10.1021/ic300733j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C46 H58 N5 O Rh'
_chemical_formula_weight         799.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.7449(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   45.474(2)
_cell_length_b                   8.9507(5)
_cell_length_c                   23.6102(12)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.33
_cell_volume                     8259.3(7)
_computing_cell_refinement       'Bruker SMART APEX2/SAINT'
_computing_data_collection       'Bruker SMART APEX2'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega'
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46503
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         9798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0307P)^2^+9.1384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                8037
_reflns_number_total             9798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300733j_si_002_1.cif
_cod_data_source_block           (dpp-nacnacCH3)Rh(phdi)(1a)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_original_cell_volume        8259.3(8)
_cod_database_code               4330990