Second-sphere coordination in anion binding: <i>cis</i>-diazidobis(ethylenediamine-κ^2^<i>N</i>,<i>N</i>')cobalt(III) picrate
Sharma, Raj Pal; Sharma, Rajni; Bala, Ritu; Bond, Andrew D.; Acta Crystallographica Section C 61 (2005) m272–m274; doi:10.1107/S0108270105011960

data_2014798
_publ_section_title
;
 Second-sphere coordination in anion binding:
 <i>cis</i>-diazidobis(ethylenediamine-\k^2^<i>N</i>,<i>N</i>')cobalt(III)
 picrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m272
_journal_page_last               m274
_journal_paper_doi               10.1107/S0108270105011960
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Co (C2 H8 N2)2 (N3)2] (C6 H2 N3 O7)'
_chemical_formula_moiety         'C4 H16 Co N10 + , C6 H2 N3 O7 -'
_chemical_formula_sum            'C10 H18 Co N13 O7'
_chemical_formula_weight         491.30
_chemical_name_common            'cis-Co(en)2(N3)2 picrate'
_chemical_name_systematic
;
cis-diazidobis(ethylenediamine-\k^2^N,N')cobalt(III) picrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.1229(3)
_cell_length_b                   12.0980(5)
_cell_length_c                   32.8793(12)
_cell_measurement_reflns_used    6972
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      2.65
_cell_volume                     3628.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker Nonius, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker Nonius X8 APEX-II CCD area-detector'
_diffrn_measurement_method       'thin-slice \w and \f'
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            20066
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS version 2.10; Sheldrick, 2003)  Ratio of minimum to maximum
apparent transmission = 0.855478
;
_exptl_crystal_colour            red-black
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.390
_refine_diff_density_min         -0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0559P)^2^+4.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                3930
_reflns_number_total             4649
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1132.cif
_cod_data_source_block           I
_cod_database_code               2014798
_cod_database_fobs_code          2014798