Linear Trichromium Complexes with Direct Cr to Cr Contacts. 2. Compounds with Cr3(dipyridylamide)43+ Cores
Rodolphe Clérac; F. Albert Cotton; Lee M. Daniels; Kim R. Dunbar; Carlos A. Murillo; Isabel Pascual; Inorganic Chemistry 39 (2000) 752–756; doi:10.1021/ic991022t

data_4300176
_publ_section_title
;
Linear Trichromium Complexes with Direct Cr to Cr Contacts. 2. Compounds
with Cr3(dipyridylamide)43+ Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              752
_journal_page_last               756
_journal_paper_doi               10.1021/ic991022t
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_structural     '[Cr3(N3C10H8)4Cl2][PF6].2(CH2Cl2)'
_chemical_formula_sum            'C42 H36 Cl3.5 Cr3 F6 N12 P'
_chemical_formula_weight         1133.87
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.545(2)
_cell_length_b                   21.426(4)
_cell_length_c                   20.238(4)
_cell_measurement_reflns_used    77
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      16.4
_cell_measurement_theta_min      7.3
_cell_volume                     5000.2(16)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST'
_diffrn_measurement_method       'Ellipsoid mask fitting'
_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  0.0874
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18460
_diffrn_reflns_theta_max         22.63
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         'None (area detector)'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2290
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_obs          0.0899
_refine_ls_shift/esd_max         -0.070
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+45.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2680
_refine_ls_wR_factor_obs         0.2094
_reflns_number_observed          4292
_reflns_number_total             6289
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+45.0000P] 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^)+(0.1000P)^2^+45.0000P] 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        5000.5(17)
_cod_original_formula_sum        'C42 H36 Cl3.50 Cr3 F6 N12 P'
_cod_database_code               4300176