First-Row Transition Metal-Halide Complexes Supported by a Monoanionic [N2P2] Ligand
Wayne A. Chomitz; Seth F. Mickenberg; John Arnold; Inorganic Chemistry 47 (2008) 373–380; doi:10.1021/ic701670u

data_4304205
_publ_section_title
;
First-Row Transition Metal-Halide Complexes Supported by a Monoanionic
[N2P2] Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              373
_journal_page_last               380
_journal_paper_doi               10.1021/ic701670u
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C22 H51 Br N2 Ni P2 Si'
_chemical_formula_sum            'C22 H51 Br N2 Ni P2 Si'
_chemical_formula_weight         572.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.564(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.555(3)
_cell_length_b                   11.593(2)
_cell_length_c                   14.908(3)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.2
_cell_volume                     2858.3(9)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      156(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15911
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.15
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.242
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                3974
_reflns_number_total             5824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701670u-file004.cif
_cod_data_source_block           wac5023xs
_cod_original_cell_volume        2858.4(8)
_cod_database_code               4304205