Atom Transfer as a Preparative Tool in Coordination Chemistry. Synthesis and Characterization of Cr(V) Nitrido Complexes of Bidentate Ligands
Torben Birk; Jesper Bendix; Inorganic Chemistry 42 (2003) 7608–7615; doi:10.1021/ic034777f

data_4312506
_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
;
 Atom Transfer as a Preparative Tool in Coordination Chemistry. Synthesis
 and Characterization of Cr(V) Nitrido Complexes of Bidentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7615
_journal_paper_doi               10.1021/ic034777f
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Local laboratory'
_chemical_formula_iupac          'Cr(N)(S2 C N C4 H8)2'
_chemical_formula_moiety         'C10 H16 Cr N3 S4 '
_chemical_formula_sum            'C10 H16 Cr N3 S4'
_chemical_formula_weight         358.511
_chemical_name_systematic
;
 bis-pyrrolidinedithiocarbamate-nitridochromium(V)
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 106.528(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8592(14)
_cell_length_b                   8.5575(5)
_cell_length_c                   11.8267(12)
_cell_measurement_reflns_used    28585
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      34.95
_cell_measurement_theta_min      1.43
_cell_volume                     1441.7(2)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'EvalCCD (Duisenberg, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       KappaCCD
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53523
_diffrn_reflns_theta_full        34.95
_diffrn_reflns_theta_max         34.95
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            Orange-brown
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.937
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         6327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0289P)^2^+1.8945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                5383
_reflns_number_total             6327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034777fsi20030707_095115_3.cif
_cod_data_source_block           pyrdtc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C10 H16 Cr N3 S4 '
_cod_database_code               4312506