#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/22/7002297.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002297
loop_
_publ_author_name
'Sengupta, Oindrila'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 Three-component assembly of a metal--inorganic 3D Co(ii) polymer
 containing bridging hydrazine
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7599
_journal_page_last               7601
_journal_paper_doi               10.1039/b907204g
_journal_year                    2009
_chemical_formula_sum            'Co3 H8 N22'
_chemical_formula_weight         493.07
_space_group_IT_number           14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8472(8)
_cell_length_b                   7.1125(6)
_cell_length_c                   10.5241(8)
_cell_measurement_temperature    293(2)
_cell_volume                     729.11(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6077
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    3.420
_exptl_absorpt_correction_T_max  0.5337
_exptl_absorpt_correction_T_min  0.4075
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_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/[σ²(Fo²)+(0.0275P)²+0.0393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                1639
_reflns_number_total             1746
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b907204g.txt
_cod_data_source_block           Comp_1
_cod_original_formula_sum        'H8 Co3 N22'
_cod_database_code               7002297
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.623864(19) 0.04874(3) 0.921009(19) 0.01491(7) Uani 1 1 d . . .
Co2 Co 1.0000 0.0000 1.0000 0.01482(8) Uani 1 2 d S . .
N1 N 0.44717(13) 0.17568(18) 0.97797(13) 0.0226(3) Uani 1 1 d . . .
N2 N 0.38541(13) 0.31141(18) 0.93371(13) 0.0212(3) Uani 1 1 d . . .
N3 N 0.32664(18) 0.4407(2) 0.89105(18) 0.0412(4) Uani 1 1 d . . .
N4 N 0.74746(13) 0.15503(19) 1.08862(12) 0.0188(3) Uani 1 1 d . . .
H4A H 0.7042(19) 0.248(3) 1.1165(17) 0.025(5) Uiso 1 1 d . . .
H4B H 0.7647(19) 0.060(3) 1.1496(19) 0.024(5) Uiso 1 1 d . . .
N5 N 0.88023(13) 0.22394(19) 1.06329(13) 0.0192(3) Uani 1 1 d . . .
H5A H 0.920(2) 0.291(3) 1.1285(19) 0.029(5) Uiso 1 1 d . . .
H5B H 0.8640(19) 0.305(3) 1.0018(18) 0.024(5) Uiso 1 1 d . . .
N6 N 0.81233(13) -0.08451(19) 0.88168(12) 0.0214(3) Uani 1 1 d . . .
N7 N 0.81899(12) -0.14163(17) 0.77613(12) 0.0178(3) Uani 1 1 d . . .
N9 N 0.51624(15) -0.03965(19) 0.74067(14) 0.0271(3) Uani 1 1 d . . .
N10 N 0.48328(13) -0.18892(18) 0.69867(12) 0.0196(3) Uani 1 1 d . . .
N11 N 0.44646(15) -0.3352(2) 0.65578(13) 0.0280(3) Uani 1 1 d . . .
N8 N 0.82528(14) -0.1938(2) 0.67344(13) 0.0277(3) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 80.34(5) 3_657 . ?
N1 Co1 N9 93.89(6) 3_657 . ?
N1 Co1 N9 93.21(6) . . ?
N1 Co1 N4 92.46(5) 3_657 . ?
N1 Co1 N4 90.44(5) . . ?
N9 Co1 N4 173.13(5) . . ?
N1 Co1 N8 171.65(5) 3_657 2_656 ?
N1 Co1 N8 91.38(5) . 2_656 ?
N9 Co1 N8 87.66(5) . 2_656 ?
N4 Co1 N8 86.43(5) . 2_656 ?
N1 Co1 N6 97.02(5) 3_657 . ?
N1 Co1 N6 174.62(5) . . ?
N9 Co1 N6 91.64(5) . . ?
N4 Co1 N6 84.98(5) . . ?
N8 Co1 N6 91.13(5) 2_656 . ?
N11 Co2 N11 180.0 2_656 4_656 ?
N11 Co2 N5 92.27(5) 2_656 . ?
N11 Co2 N5 87.73(5) 4_656 . ?
N11 Co2 N5 87.73(5) 2_656 3_757 ?
N11 Co2 N5 92.27(5) 4_656 3_757 ?
N5 Co2 N5 180.000(1) . 3_757 ?
N11 Co2 N6 90.18(5) 2_656 3_757 ?
N11 Co2 N6 89.82(5) 4_656 3_757 ?
N5 Co2 N6 94.44(5) . 3_757 ?
N5 Co2 N6 85.56(5) 3_757 3_757 ?
N11 Co2 N6 89.82(5) 2_656 . ?
N11 Co2 N6 90.18(5) 4_656 . ?
N5 Co2 N6 85.56(5) . . ?
N5 Co2 N6 94.44(5) 3_757 . ?
N6 Co2 N6 180.0 3_757 . ?
N2 N1 Co1 128.55(11) . 3_657 ?
N2 N1 Co1 128.54(11) . . ?
Co1 N1 Co1 99.66(5) 3_657 . ?
N3 N2 N1 179.74(19) . . ?
N5 N4 Co1 112.77(9) . . ?
N5 N4 H4A 107.9(13) . . ?
Co1 N4 H4A 107.7(12) . . ?
N5 N4 H4B 107.0(12) . . ?
Co1 N4 H4B 109.8(12) . . ?
H4A N4 H4B 111.7(16) . . ?
N4 N5 Co2 110.85(9) . . ?
N4 N5 H5A 110.1(12) . . ?
Co2 N5 H5A 116.6(12) . . ?
N4 N5 H5B 106.8(12) . . ?
Co2 N5 H5B 108.3(12) . . ?
H5A N5 H5B 103.5(18) . . ?
N7 N6 Co2 118.21(10) . . ?
N7 N6 Co1 119.33(10) . . ?
Co2 N6 Co1 116.81(6) . . ?
N8 N7 N6 178.87(16) . . ?
N10 N9 Co1 132.46(12) . . ?
N11 N10 N9 177.92(16) . . ?
N10 N11 Co2 133.17(12) . 2_646 ?
N7 N8 Co1 138.28(12) . 2_646 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.0942(13) 3_657 ?
Co1 N1 2.1232(13) . ?
Co1 N9 2.1284(14) . ?
Co1 N4 2.1293(13) . ?
Co1 N8 2.1768(14) 2_656 ?
Co1 N6 2.1770(12) . ?
Co2 N11 2.1432(14) 2_656 ?
Co2 N11 2.1432(14) 4_656 ?
Co2 N5 2.1453(13) . ?
Co2 N5 2.1453(13) 3_757 ?
Co2 N6 2.1567(13) 3_757 ?
Co2 N6 2.1567(13) . ?
N1 N2 1.1982(18) . ?
N1 Co1 2.0942(13) 3_657 ?
N2 N3 1.1426(19) . ?
N4 N5 1.4570(18) . ?
N4 H4A 0.86(2) . ?
N4 H4B 0.93(2) . ?
N5 H5A 0.88(2) . ?
N5 H5B 0.86(2) . ?
N6 N7 1.1936(17) . ?
N7 N8 1.1529(17) . ?
N9 N10 1.1772(19) . ?
N10 N11 1.1703(19) . ?
N11 Co2 2.1432(14) 2_646 ?
N8 Co1 2.1768(13) 2_646 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A N3 0.86(2) 2.24(2) 2.982(2) 145.0(16) 3_667
N4 H4B N11 0.93(2) 2.395(19) 3.0179(19) 124.3(15) 4_656
N4 H4B N3 0.93(2) 2.52(2) 3.236(2) 133.6(14) 4_666
N5 H5A N9 0.88(2) 2.26(2) 3.0963(19) 159.8(17) 4_666
N5 H5B N8 0.86(2) 2.422(19) 3.0274(19) 127.5(15) 2_656
