[Cr(N)Cl4]2-: A Simple Nitrido Complex Synthesized by Nitrogen-Atom Transfer
Jesper Bendix; Journal of the American Chemical Society 125 (2003) 13348–13349; doi:10.1021/ja0371000

data_4114317
_publ_contact_author
; 
Jesper Bendix
University of Copenhagen
Department of Chemistry 
Universitetsparken 5 
DK-2100
Denmark
;
_publ_contact_author_email       Bendix@kiku.dk
_publ_contact_author_fax         '+45 35320133'
_publ_contact_author_phone       '+45 35320101'
_publ_section_title
;
 [Cr(N)Cl4]2-: A Simple Nitrido Complex Synthesized by Nitrogen-Atom
 Transfer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13348
_journal_page_last               13349
_journal_paper_doi               10.1021/ja0371000
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '2(C4 H12 N), Cl4 Cr N, H2 O'
_chemical_formula_sum            'C8 H26 Cl4 Cr N3 O'
_chemical_formula_weight         374.12
_chemical_name_systematic
; 
bis(tetramethylammonium)tetrachloronitridochromate(V)hydrate
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2003-06-20   text and data added, srw 
2003-06-24   last corrections, JB
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3488(14)
_cell_length_b                   12.3488(14)
_cell_length_c                   12.3488(14)
_cell_measurement_temperature    122(1)
_cell_volume                     1883.1(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      ??
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  jbas
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0071
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5184
_diffrn_reflns_theta_full        21.90
_diffrn_reflns_theta_max         21.90
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_T_max  0.8802
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             780
_exptl_crystal_id                jbcrncl4
_exptl_crystal_preparation
; 
?
;
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         84
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1406P)^2^+7.4873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                82
_reflns_number_total             84
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0371000si20030707_045246.cif
_cod_data_source_block           jbcrncl4
_cod_original_sg_symbol_Hall     '-F 4 2 3 '
_cod_database_code               4114317