Coordination of bis(azol-1-yl)methane-based bisphosphines towards Ru(II), Rh(I), Pd(II) and Pt(II): synthesis, structural and catalytic studies.
Bhat, Sajad A.; Pandey, Madhusudan K.; Mague, Joel T.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 46 (2016) 227–241; doi:10.1039/c6dt04094b

data_7041237
_publ_section_title
;
 Coordination of bis(azol-1-yl)methane-based bisphosphines towards Ru(II),
 Rh(I), Pd(II) and Pt(II): synthesis, structural and catalytic studies.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              227
_journal_page_last               241
_journal_paper_doi               10.1039/c6dt04094b
_journal_volume                  46
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C47 H50 N4 P2 Rh2, 2(B F4)'
_chemical_formula_sum            'C47 H50 B2 F8 N4 P2 Rh2'
_chemical_formula_weight         1112.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-10-23 deposited with the CCDC.
2016-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.8490(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8580(3)
_cell_length_b                   11.7581(3)
_cell_length_c                   13.3446(3)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.189
_cell_measurement_theta_min      3.500
_cell_volume                     2354.80(9)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2013)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2013)'
_computing_data_reduction        '<i>SAINT</i>  (Bruker, 2013)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXT</i> (Bruker AXS 2013c)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17112
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         72.182
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'INCOATEC I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    6.912
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '<i>SADABS</i> (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.757
_exptl_transmission_factor_min   0.453
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1854 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack, 2004).
;
_refine_ls_abs_structure_Flack   0.027(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+3.9606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                4209
_reflns_number_total             4256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04094b2.cif
_cod_data_source_block           compound14_MSB686_0m_b
_cod_depositor_comments
'Adding full bibliography for 7041235--7041247.cif.'
_cod_database_code               7041237
_shelx_estimated_absorpt_t_min   0.467
_shelx_estimated_absorpt_t_max   0.819
_shelxl_version_number           2013-4
_shelx_res_checksum              42093