Achiral and Chiral PNP-Pincer Ligands with a Carbazole Backbone: Coordination Chemistry with d8 Transition Metals
Nora Grüger; Lara-Isabel Rodríguez; Hubert Wadepohl; Lutz H. Gade; Inorganic Chemistry 52 (2013) 2050–2059; doi:10.1021/ic302454n

data_4333884
_publ_section_title
;
 Achiral and Chiral PNP-Pincer Ligands with a Carbazole Backbone:
 Coordination Chemistry with d8 Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2050
_journal_page_last               2059
_journal_paper_doi               10.1021/ic302454n
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C47 H47 Br Cl3 N Ni P2'
_chemical_formula_weight         932.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ng20
_audit_creation_method           SHELXL-97
_audit_update_record             'Mon Jun 18 14:46:50 CEST 2012'
_cell_angle_alpha                62.554(11)
_cell_angle_beta                 76.346(10)
_cell_angle_gamma                68.730(13)
_cell_formula_units_Z            2
_cell_length_a                   12.639(6)
_cell_length_b                   14.010(7)
_cell_length_c                   14.816(8)
_cell_measurement_reflns_used    5529
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.42
_cell_volume                     2162.1(19)
_computing_cell_refinement
;
SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT (Bruker AXS, 1997-2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2011 (Giacovazzo et al., 2011)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40954
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'fine-focus sealed tube (Mo)'
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  0.9605
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.229
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8874
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+5.4856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                6432
_reflns_number_total             8874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302454n_si_002_4.cif
_cod_data_source_block           complex_9b
_cod_database_code               4333884
_audit_block_refno               1447
_audit_block_usercomment         ng198-03