#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:14:20 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224448 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/94/7049429.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_7049429
loop_
_publ_author_name
'Zhu, Jiaxing'
'Chen, Junye'
'Qiu, Tianze'
'Deng, Mingli'
'Zheng, Qingshu'
'Chen, Zhenxia'
'Ling, Yun'
'Zhou, Yaming'
_publ_section_title
;
 Cobalt substitution in a flexible metal-organic framework: modulating a
 soft paddle-wheel unit for tunable gate-opening adsorption.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7100
_journal_page_last               7104
_journal_paper_doi               10.1039/c9dt00115h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H10 Co N5 O8 Zn, C2 H8 N, 6.5(H2 O)'
_chemical_formula_sum            'C20 H31 Co N6 O14.5 Zn'
_chemical_formula_weight         711.81
_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'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-03-02 deposited with the CCDC.    2019-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.5710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.414(2)
_cell_length_b                   19.927(2)
_cell_length_c                   12.8456(16)
_cell_measurement_reflns_used    7128
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.84
_cell_volume                     3579.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10720
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.149
_diffrn_reflns_theta_max         25.149
_diffrn_reflns_theta_min         1.779
_diffrn_source                   'fine-focus fiber'
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0310P)²+22.4345P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2959
_reflns_number_total             3284
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00115h2.cif
_cod_data_source_block           MAC-6-Zn1Co1
_cod_depositor_comments
'Adding full bibliography for 7049426--7049429.cif.'
_cod_original_cell_volume        3579.9(8)
_cod_original_formula_sum        'C20 H31 Co N6 O14.50 Zn'
_cod_database_code               7049429
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.754
_shelx_estimated_absorpt_t_max   0.841
_exptl_absorpt_special_details   none
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn1 Zn 0.09201(4) 0.000000 0.12869(5) 0.01455(16) Uani 0.5 2 d S T P
Co1 Co 0.09201(4) 0.000000 0.12869(5) 0.01455(16) Uani 0.5 2 d S T P
Zn2 Zn 0.500000 0.09015(3) 0.500000 0.01667(16) Uani 0.5 2 d S T P
Co2 Co 0.500000 0.09015(3) 0.500000 0.01667(16) Uani 0.5 2 d S T P
C1 C 0.0371(2) 0.09740(17) -0.0964(3) 0.0233(7) Uani 1 1 d . . .
C2 C 0.0713(2) 0.15895(18) -0.1238(3) 0.0272(8) Uani 1 1 d . . .
C3 C 0.0112(2) 0.19542(19) -0.2384(4) 0.0302(8) Uani 1 1 d . . .
H3 H -0.050550 0.180487 -0.301726 0.036 Uiso 1 1 calc R U .
C4 C 0.0445(2) 0.2539(2) -0.2567(4) 0.0342(9) Uani 1 1 d . . .
C5 C 0.1383(2) 0.27483(19) -0.1625(4) 0.0335(9) Uani 1 1 d . . .
H5 H 0.160013 0.314191 -0.175805 0.040 Uiso 1 1 calc R U .
C6 C 0.2000(2) 0.23838(18) -0.0493(3) 0.0283(8) Uani 1 1 d . . .
C7 C 0.1639(2) 0.18083(18) -0.0304(3) 0.0275(8) Uani 1 1 d . . .
H7 H 0.202584 0.156753 0.046368 0.033 Uiso 1 1 calc R U .
C8 C -0.0169(3) 0.2975(2) -0.3751(4) 0.0408(11) Uani 1 1 d . . .
C9 C 0.2925(2) 0.05368(15) 0.3349(3) 0.0155(6) Uani 1 1 d . . .
N1 N 0.2325(2) 0.000000 0.2805(3) 0.0134(7) Uani 1 2 d S T P
N2 N 0.38333(17) 0.03521(12) 0.4140(2) 0.0157(5) Uani 1 1 d . . .
N3 N 0.26266(19) 0.11823(14) 0.3072(3) 0.0249(7) Uani 1 1 d . . .
H3A H 0.303743 0.150329 0.341814 0.030 Uiso 1 1 calc R U .
H3B H 0.202593 0.127156 0.255004 0.030 Uiso 1 1 calc R U .
O1 O 0.09362(16) 0.07008(12) 0.0120(2) 0.0282(6) Uani 1 1 d . . .
O2 O -0.04675(17) 0.07668(13) -0.1834(2) 0.0308(6) Uani 1 1 d . . .
O3 O 0.01912(19) 0.35502(14) -0.3637(3) 0.0452(8) Uani 1 1 d . . .
O4 O -0.0955(2) 0.27818(16) -0.4689(3) 0.0598(11) 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
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'
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'
Zn Zn 0.2839 1.4301 '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
N1 Zn1 O2 99.34(10) . 5
N1 Zn1 O2 99.34(10) . 2
O2 Zn1 O2 97.82(16) 5 2
N1 Zn1 O1 99.68(10) . 6
O2 Zn1 O1 85.30(11) 5 6
O2 Zn1 O1 159.95(10) 2 6
N1 Zn1 O1 99.68(10) . .
O2 Zn1 O1 159.95(10) 5 .
O2 Zn1 O1 85.30(11) 2 .
O1 Zn1 O1 85.30(15) 6 .
N1 Zn1 Zn1 165.57(11) . 5
O2 Zn1 Zn1 90.09(7) 5 5
O2 Zn1 Zn1 90.09(7) 2 5
O1 Zn1 Zn1 70.05(7) 6 5
O1 Zn1 Zn1 70.05(7) . 5
O3 Zn2 O3 110.5(2) 8_556 7
O3 Zn2 N2 112.91(12) 8_556 .
O3 Zn2 N2 104.17(11) 7 .
O3 Zn2 N2 104.18(11) 8_556 2_656
O3 Zn2 N2 112.91(12) 7 2_656
N2 Zn2 N2 112.39(14) . 2_656
O1 C1 O2 124.6(3) . .
O1 C1 C2 117.3(3) . .
O2 C1 C2 118.1(3) . .
C7 C2 C3 120.2(3) . .
C7 C2 C1 118.4(3) . .
C3 C2 C1 121.4(3) . .
C4 C3 C2 119.4(3) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.8(3) . .
C3 C4 C8 122.7(3) . .
C5 C4 C8 117.5(3) . .
C6 C5 C4 121.8(3) . .
C6 C5 H5 119.1 . .
C4 C5 H5 119.1 . .
C5 C6 C7 117.5(3) . .
C5 C6 C6 120.7(4) . 7
C7 C6 C6 121.8(4) . 7
C2 C7 C6 121.3(3) . .
C2 C7 H7 119.4 . .
C6 C7 H7 119.4 . .
O4 C8 O3 125.5(3) . .
O4 C8 C4 120.9(3) . .
O3 C8 C4 113.5(3) . .
N2 C9 N3 124.2(3) . .
N2 C9 N1 112.1(3) . .
N3 C9 N1 123.7(3) . .
C9 N1 C9 103.5(3) 6 .
C9 N1 Zn1 127.70(17) 6 .
C9 N1 Zn1 127.70(17) . .
C9 N2 N2 106.14(17) . 6
C9 N2 Zn2 129.6(2) . .
N2 N2 Zn2 123.80(7) 6 .
C9 N3 H3A 120.0 . .
C9 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
C1 O1 Zn1 139.5(2) . .
C1 O2 Zn1 114.9(2) . 5
C8 O3 Zn2 127.1(3) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.026(3) .
Zn1 O2 2.027(2) 5
Zn1 O2 2.027(2) 2
Zn1 O1 2.061(2) 6
Zn1 O1 2.061(2) .
Zn1 Zn1 2.9283(11) 5
Zn2 O3 1.917(3) 8_556
Zn2 O3 1.917(3) 7
Zn2 N2 1.968(2) .
Zn2 N2 1.968(2) 2_656
C1 O1 1.253(4) .
C1 O2 1.268(4) .
C1 C2 1.495(5) .
C2 C7 1.386(5) .
C2 C3 1.398(5) .
C3 C4 1.382(5) .
C3 H3 0.9300 .
C4 C5 1.397(5) .
C4 C8 1.509(5) .
C5 C6 1.391(5) .
C5 H5 0.9300 .
C6 C7 1.398(5) .
C6 C6 1.490(6) 7
C7 H7 0.9300 .
C8 O4 1.228(5) .
C8 O3 1.272(5) .
C9 N2 1.324(4) .
C9 N3 1.353(4) .
C9 N1 1.362(4) .
N2 N2 1.403(5) 6
N3 H3A 0.8600 .
N3 H3B 0.8600 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.500 -0.011 1007 277 ' '
2 0.324 0.000 -0.176 988 274 ' '
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 7 0 7.319
0 8 0 8.202
-6 0 4 7.535
0 0 4 7.920
-1 1 4 7.216
-1 3 4 7.779
-2 4 4 7.777
-4 0 5 7.951
