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_7027357
_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            'C34 H49 Cr N4 P'
_chemical_formula_weight         596.74
_chemical_name_systematic
; 
 ? 
;
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.884(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9487(7)
_cell_length_b                   18.5847(7)
_cell_length_c                   18.7972(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      10.79
_cell_volume                     3475.1(3)
_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      203(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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5475
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.334
_exptl_absorpt_correction_T_max  0.5405
_exptl_absorpt_correction_T_min  0.2790
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.00042(11)
_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   1.039
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_obs          0.0535
_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^)+(0.0816P)^2^+1.4865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1469
_refine_ls_wR_factor_obs         0.1327
_reflns_number_observed          4076
_reflns_number_total             5141
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901790isup1.cif
_cod_data_source_block           VG9861
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+1.4865P] 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^)+(0.0816P)^2^+1.4865P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C34 H49 N4 P Cr'
_cod_database_code               7027357