Bis(imino)phosphanes: Synthesis and Coordination Chemistry
van Dijk, Tom; Rong, Mark K.; Borger, Jaap E.; Nieger, Martin; Slootweg, J. Chris; Lammertsma, Koop; Organometallics 35 (2016) 827–; doi:10.1021/acs.organomet.6b00063

data_4088404
_publ_section_title
;
 Bis(imino)phosphanes: Synthesis and Coordination Chemistry
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              827
_journal_paper_doi               10.1021/acs.organomet.6b00063
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C36 H49 Cl N P Rh2, C H2 Cl2'
_chemical_formula_sum            'C37 H51 Cl3 N P Rh2'
_chemical_formula_weight         852.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                86.78(1)
_cell_angle_beta                 87.00(1)
_cell_angle_gamma                87.00(1)
_cell_formula_units_Z            2
_cell_length_a                   10.428(1)
_cell_length_b                   11.901(1)
_cell_length_c                   14.709(1)
_cell_measurement_reflns_used    216
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     1817.8(3)
_computing_cell_refinement       EVALCCD
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in \f and \w, 2\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31559
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Shelcrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       blocks
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.4336P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7446
_reflns_number_total             8322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00063_si_003.cif
_cod_data_source_block           jcs013_compound_6
_cod_database_code               4088404
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2013-2
_shelx_res_checksum              15457