Synthesis and characterisation of 2,6-diisopropylphenylimido complexes of chromium in oxidation states IV‒VI
Chew, Kong Chin; Clegg, William; Coles, Martyn P.; Elsegood, Mark R. J.; Gibson, Vernon C.; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (1999) 2633–; doi:10.1039/a901790i

data_7027354
_publ_section_title
;
 Synthesis and characterisation of 2,6-diisopropylphenylimido complexes of
 chromium in oxidation states IV--VI
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2633
_journal_paper_doi               10.1039/a901790i
_journal_year                    1999
_chemical_formula_sum            'C36 H52 Cl Cr N3'
_chemical_formula_weight         614.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom except h1 coords refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'all non-H found by direct methods'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.707(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4714(11)
_cell_length_b                   15.411(2)
_cell_length_c                   21.493(2)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.10
_cell_volume                     3456.7(7)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14712
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       'thick plate'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0023(3)
_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   1.203
_refine_ls_goodness_of_fit_obs   1.232
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.232
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_obs          0.0588
_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^)+(0.0214P)^2^+5.2883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1248
_refine_ls_wR_factor_obs         0.1177
_reflns_number_observed          4943
_reflns_number_total             5734
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901790isup1.cif
_cod_data_source_block           vcg72
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+5.2883P] 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^)+(0.0214P)^2^+5.2883P] 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        3456.7(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027354