The pentacoordinated [Cr(CO)~5~]^2{-^} dianion in [2,2,2-crypt-K]~2~[Cr(CO)~5~] ethylenediamine monosolvate
Zhai, Jun; Xu, Li; Acta Crystallographica Section C 67 (2011) m202–m204; doi:10.1107/S0108270111018233

data_2018090
_publ_section_title
;
 The pentacoordinated [Cr(CO)~5~]^2{-^} dianion in
 [2,2,2-crypt-K]~2~[Cr(CO)~5~] ethylenediamine monosolvate
;
_journal_coeditor_code           BI3018
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m202
_journal_page_last               m204
_journal_paper_doi               10.1107/S0108270111018233
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[K (C18 H36 N2 O6)]2 [Cr (C O)5] , C2 H8 N2'
_chemical_formula_moiety
'2(C18 H36 K N2 O6 2+), C5 Cr O5 2-, C2 H8 N2'
_chemical_formula_sum            'C43 H80 Cr K2 N6 O17'
_chemical_formula_weight         1083.33
_chemical_name_systematic
;
Bis[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium(+)]
pentacarbonylchromate(2-) ethylenediamine monosolvate
;
_space_group_IT_number           1
_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
_cell_angle_alpha                63.883(7)
_cell_angle_beta                 66.841(10)
_cell_angle_gamma                86.820(13)
_cell_formula_units_Z            1
_cell_length_a                   11.034(3)
_cell_length_b                   11.741(4)
_cell_length_c                   12.818(3)
_cell_measurement_reflns_used    3395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.34
_cell_volume                     1356.9(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10684
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.283
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                5037
_reflns_number_total             7850
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3018.cif
_cod_data_source_block           I
_cod_database_code               2018090
_cod_database_fobs_code          2018090