Synthesis and reactivity of 1,8-bis(imino)carbazolide complexes of iron, cobalt and manganese
Gibson, Vernon C.; Spitzmesser, Stefan K.; White, Andrew J. P.; Williams, David J.; Dalton Transactions  (2003) 2718–; doi:10.1039/b301902k

data_7012856
_publ_section_title
;
 Synthesis and reactivity of 1,8-bis(imino)carbazolide complexes of
 iron, cobalt and manganese
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2718
_journal_paper_doi               10.1039/b301902k
_journal_year                    2003
_chemical_formula_sum            'C28 H22 Cl2 Fe N3'
_chemical_formula_weight         527.24
_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
_cell_angle_alpha                94.896(6)
_cell_angle_beta                 101.507(7)
_cell_angle_gamma                97.380(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4774(5)
_cell_length_b                   11.4602(6)
_cell_length_c                   11.7408(8)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      10.77
_cell_volume                     1231.11(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3904
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.87
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.072
_exptl_absorpt_correction_T_max  0.3237
_exptl_absorpt_correction_T_min  0.1949
_exptl_absorpt_correction_type   Ellispoidal
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prisms
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1128
_refine_ls_wR_factor_obs         0.1029
_reflns_number_observed          2962
_reflns_number_total             3649
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b301902k.txt
_cod_data_source_block           Compound_9c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1231.11(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C28 H22 N3 Cl2 Fe'
_cod_database_code               7012856