[Na(THF)2Cr(N3N)]: The First Trigonal Monopyramidal Chromium(II) Complex
Alexander C. Filippou; Sven Schneider; Gregor Schnakenburg; Inorganic Chemistry 42 (2003) 6974–6976; doi:10.1021/ic0349961

data_4312454
_publ_section_title
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 [Na(THF)2Cr(N3N)]: The First Trigonal Monopyramidal Chromium(II) Complex
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6974
_journal_page_last               6976
_journal_paper_doi               10.1021/ic0349961
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C23 H55 Cr N4 Na O2 Si3'
_chemical_formula_sum            'C23 H55 Cr N4 Na O2 Si3'
_chemical_formula_weight         578.97
_chemical_melting_point          400(2)
_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           SHELXL97
_cell_angle_alpha                87.74(3)
_cell_angle_beta                 86.56(2)
_cell_angle_gamma                64.30(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4641(19)
_cell_length_b                   11.381(3)
_cell_length_c                   15.994(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.5
_cell_volume                     1713.0(7)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.4\%,171 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11662
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.8629
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
The correction was carried out by ABSCOR (Stoe, 1997), a modification of
DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166.
In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                4829
_reflns_number_total             5958
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0349961si20030822_121428.cif
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        1713.1(6)
_cod_database_code               4312454