#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:43:17 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231588 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/60/4346030.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_4346030
loop_
_publ_author_name
'Chen, Di-Ming'
'Ma, Xiao-Zhou'
'Zhang, Xue-Jing'
'Xu, Na'
'Cheng, Peng'
_publ_section_title
;
 Switching a 2D Co(II) layer to a 3D Co7-cluster-based metal-organic
 framework: syntheses, crystal structures, and magnetic properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2976
_journal_page_last               2982
_journal_paper_doi               10.1021/acs.inorgchem.5b00074
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'0.5(C20 H16 Cl2 Co2 N6 O4), H3 O, 0.5(H4 O2), 0.67(O)'
_chemical_formula_sum            'C10 H13 Cl Co N3 O4.5'
_chemical_formula_weight         341.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.467(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.687(2)
_cell_length_b                   7.2468(7)
_cell_length_c                   11.5369(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1402.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2631
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1344
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0637
_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/[σ²(Fo²)+(0.0807P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                957
_reflns_number_total             1344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00074_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        1402.6(2)
_cod_original_formula_sum        'C10 H13 Cl Co N3 O4.50'
_cod_database_code               4346030
_olex2_refinement_description
;
1. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H1AA(0.5) H0AA(0.5) H0AB(0.5) O1(0.33)
 Fixed U12: N3(0) C5(0) C6(0) C7(0) C12(0) Cl1(0) O1AA(0) O0AA(0)
 Fixed U23: N3(0) C5(0) C6(0) C7(0) C12(0) Cl1(0) O1AA(0) O0AA(0)
 Fixed Uiso: H7A(0.019) H7B(0.019) H9(0.021) H10(0.022) H11(0.024) H1AA(0.059)
 H1AB(0.059) H0AA(0.059) H0AB(0.059)
 Fixed X: Co1(0.25) H7A(0.0278) H7B(0.0278) H9(0.1981) H10(0.1603) H11(0.1044)
 H1AA(-0.0682) H1AB(-0.1163) H0AA(0.0939) H0AB(0.043)
 Fixed Y: Co1(0.25) N3(0) C5(0) C6(0) C7(0) H7A(0.1085) H7B(-0.1085)
 H9(0.2697) H10(0.2757) H11(0.2762) C12(0) Cl1(0.5) O1AA(0.5) O0AA(0.5)
 H1AA(0.4762) H1AB(0.5682) H0AA(0.6074) H0AB(0.4633)
 Fixed Z: Co1(0) H7A(0.6861) H7B(0.6861) H9(0.2533) H10(0.4167) H11(0.5738)
 H1AA(0.3351) H1AB(0.2314) H0AA(0.2676) H0AB(0.2715)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z'
5 '-x, -y, -z'
6 'x, -y, z'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z'
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.2500 0.2500 0.0000 0.0121(4) Uani 1 d . . 2 S T P
N3 N 0.1904(4) 0.0000 0.2963(5) 0.0148(16) Uani 1 d . . 2 S T P
N4 N 0.2230(3) 0.0954(6) 0.1367(3) 0.0129(11) Uani 1 d . . 1 . . .
C5 C 0.1625(5) 0.0000 0.3994(6) 0.0142(19) Uani 1 d . . 2 S T P
C6 C 0.1272(5) 0.0000 0.8154(7) 0.0148(19) Uani 1 d . . 2 S T P
C7 C 0.0610(5) 0.0000 0.6928(6) 0.0156(19) Uani 1 d . . 2 S T P
H7A H 0.0278 0.1085 0.6861 0.019 Uiso 0.50 calc . . 1 R . .
H7B H 0.0278 -0.1085 0.6861 0.019 Uiso 0.50 calc . . 1 R . .
C9 C 0.2030(3) 0.1474(9) 0.2323(5) 0.0177(14) Uani 1 d . . 1 . . .
H9 H 0.1981 0.2697 0.2533 0.021 Uiso 1 calc . . 1 R . .
C10 C 0.1482(4) 0.1648(9) 0.4475(5) 0.0186(15) Uani 1 d . . 1 . . .
H10 H 0.1603 0.2757 0.4167 0.022 Uiso 1 calc . . 1 R . .
C11 C 0.1154(4) 0.1648(9) 0.5426(5) 0.0201(15) Uani 1 d . . 1 . . .
H11 H 0.1044 0.2762 0.5738 0.024 Uiso 1 calc . . 1 R . .
C12 C 0.0992(5) 0.0000 0.5908(6) 0.0144(19) Uani 1 d . . 2 S T P
O3 O 0.1526(2) -0.1558(5) 0.8608(3) 0.0164(10) Uani 1 d . . 1 . . .
Cl1 Cl 0.16784(13) 0.5000 0.03536(16) 0.0174(5) Uani 1 d . . 2 S T P
O1AA O -0.0758(4) 0.5000 0.2611(5) 0.0290(17) Uani 1 d . . 2 DS T P
O0AA O 0.0783(4) 0.5000 0.2409(5) 0.0397(19) Uani 1 d . . 2 S T P
H1AA H -0.0682 0.4762 0.3351 0.059 Uiso 0.50 d . . 1 DG . .
H1AB H -0.1163 0.5682 0.2314 0.059 Uiso 1 d . . 1 DG . .
H0AA H 0.0939 0.6074 0.2676 0.059 Uiso 0.50 d . . 1 G . .
H0AB H 0.0430 0.4633 0.2715 0.059 Uiso 0.50 d . . 1 G . .
O1 O 0.010(3) 0.894(2) 0.015(5) 0.065(9) Uani 0.33 d A -1 1 . U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
N4 Co1 N4 179.999(1) . 7
N4 Co1 Cl1 91.07(13) . 7
N4 Co1 Cl1 88.93(13) . .
N4 Co1 Cl1 88.93(13) 7 7
N4 Co1 Cl1 91.07(13) 7 .
O3 Co1 N4 94.30(15) 6_554 .
O3 Co1 N4 85.70(15) 6_554 7
O3 Co1 N4 85.70(15) 4_556 .
O3 Co1 N4 94.30(15) 4_556 7
O3 Co1 O3 180.000(1) 4_556 6_554
O3 Co1 Cl1 88.93(12) 4_556 7
O3 Co1 Cl1 91.07(12) 4_556 .
O3 Co1 Cl1 91.07(12) 6_554 7
O3 Co1 Cl1 88.93(12) 6_554 .
Cl1 Co1 Cl1 180.0 7 .
C9 N3 C5 127.9(3) 6 .
C9 N3 C5 127.9(3) . .
C9 N3 C9 103.9(6) . 6
N4 N4 Co1 122.09(12) 6 .
C9 N4 Co1 131.3(4) . .
C9 N4 N4 106.6(3) . 6
C10 C5 N3 119.6(4) 6 .
C10 C5 N3 119.6(4) . .
C10 C5 C10 120.8(7) . 6
O3 C6 C7 116.9(3) . .
O3 C6 C7 116.9(3) 6 .
O3 C6 O3 126.2(7) 6 .
C6 C7 C12 108.4(6) . .
N4 C9 N3 111.4(5) . .
C5 C10 C11 119.6(6) . .
C12 C11 C10 120.5(6) . .
C11 C12 C7 120.4(4) 6 .
C11 C12 C7 120.4(4) . .
C11 C12 C11 119.1(7) . 6
C6 O3 Co1 135.8(4) . 4_546
Co1 Cl1 Co1 96.08(8) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N4 2.109(4) 7
Co1 N4 2.109(4) .
Co1 O3 2.064(3) 4_556
Co1 O3 2.064(3) 6_554
Co1 Cl1 2.4364(15) 7
Co1 Cl1 2.4364(15) .
N3 C5 1.424(10) .
N3 C9 1.357(7) 6
N3 C9 1.357(7) .
N4 N4 1.383(9) 6
N4 C9 1.316(7) .
C5 C10 1.374(7) .
C5 C10 1.374(7) 6
C6 C7 1.524(10) .
C6 O3 1.266(5) .
C6 O3 1.266(5) 6
C7 C12 1.531(11) .
C10 C11 1.394(8) .
C11 C12 1.386(7) .
C12 C11 1.386(7) 6
O3 Co1 2.064(3) 4_546
Cl1 Co1 2.4364(15) 4
