Low valent chromium complexes bearing N,O-chelating pyridyl-enolate ligands [OC(Bu^t^)(=2-CHN~5~H~3~Me-x)]^-^ (x = 3-6)
Gibson, Vernon C.; Newton, Claire; Redshaw, Carl; Solan, Gregory A.; White, Andrew J. P.; Williams, David J.; Dalton Transactions  (2003) 4612–4617; doi:10.1039/b308881m

data_7013485
_publ_section_title
;
 Low valent chromium complexes bearing N,O-chelating pyridyl-enolate
 ligands [OC(Bu^t^)(=2-CHN~5~H~3~Me-x)]^-^ (x = 3-6)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4612
_journal_page_last               4617
_journal_paper_doi               10.1039/b308881m
_journal_year                    2003
_chemical_formula_sum            'C36 H48 Cr N3 O3'
_chemical_formula_weight         622.77
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 90.94(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.957(2)
_cell_length_b                   18.642(3)
_cell_length_c                   16.593(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.44
_cell_measurement_theta_min      10.70
_cell_volume                     3388.8(10)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5298
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         2.37
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.069
_exptl_absorpt_correction_T_max  0.8937
_exptl_absorpt_correction_T_min  0.2862
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Orange/red
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       'prismatic needles'
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_coef       0.0012(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   1.031
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_obs          0.0881
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2414
_refine_ls_wR_factor_obs         0.2169
_reflns_number_observed          4237
_reflns_number_total             5298
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b308881m.txt
_cod_data_source_block           Compound_3
_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 2.4.1 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^)+(0.1880P)^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^)+(0.1880P)^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_sg_symbol_H-M      Pn
_cod_original_formula_sum        'C36 H48 N3 O3 Cr'
_cod_database_code               7013485