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_4304203
_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 Cl2 Cr N2 P2 Si'
_chemical_formula_sum            'C22 H51 Cl2 Cr N2 P2 Si'
_chemical_formula_weight         556.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.665(10)
_cell_angle_beta                 103.110(10)
_cell_angle_gamma                108.597(10)
_cell_formula_units_Z            2
_cell_length_a                   8.323(5)
_cell_length_b                   11.887(7)
_cell_length_c                   16.425(10)
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      21.8
_cell_measurement_theta_min      2.6
_cell_volume                     1440.5(15)
_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      163(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0960
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9350
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.33
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1205
_reflns_number_gt                3757
_reflns_number_total             5722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701670u-file002.cif
_cod_data_source_block           wac4050xs
_cod_original_cell_volume        1440.4(15)
_cod_database_code               4304203