#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:49:17 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/11/7231159.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_7231159
loop_
_publ_author_name
'Shrivastava, Ashutosh'
'Negi, Lalita'
'Das, Dinabandhu'
_publ_section_title
;
 Area negative thermal expansion in a mixed metal mixed organic MOF:
 “elevator-platform” mechanism induced by O--H⋯O
 hydrogen bonding
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4719
_journal_paper_doi               10.1039/C8CE00939B
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C22 H26 Co N2 O20 Zn2, 4(H2 O)'
_chemical_formula_sum            'C22 H34 Co N2 O24 Zn2'
_chemical_formula_weight         900.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-07-02 deposited with the CCDC.
2018-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.6190(10)
_cell_angle_beta                 89.025(2)
_cell_angle_gamma                83.164(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5387(3)
_cell_length_b                   10.1927(4)
_cell_length_c                   10.7387(4)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.72
_cell_volume                     818.52(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX III'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-Seed (Barbour 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-III CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32459
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.712
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             459
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.260
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6098
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0095(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0227
_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)+(0.0254P)²+0.9884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3857
_reflns_number_total             4071
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00939b2.cif
_cod_data_source_block           1_200K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7231150--7231161.cif.
;
_cod_database_code               7231159
_shelx_shelxl_version_number     2018/3
_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   0.533
_shelx_estimated_absorpt_t_max   0.617
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.2529(2) 0.56939(15) 0.45284(14) 0.0109(3) Uani 1 1 d . . .
C2 C 0.2262(2) 0.46417(15) 0.37910(14) 0.0113(3) Uani 1 1 d . . .
H2 H 0.197194 0.480384 0.293670 0.014 Uiso 1 1 calc R U .
C3 C 0.2419(2) 0.33529(15) 0.43008(14) 0.0098(3) Uani 1 1 d . . .
C4 C 0.2831(2) 0.31197(15) 0.55574(14) 0.0107(3) Uani 1 1 d . . .
H4 H 0.294760 0.224187 0.590527 0.013 Uiso 1 1 calc R U .
C5 C 0.3072(2) 0.41674(15) 0.63060(14) 0.0098(3) Uani 1 1 d . . .
C6 C 0.2934(2) 0.54468(15) 0.57811(15) 0.0116(3) Uani 1 1 d . . .
H6 H 0.311961 0.616098 0.628557 0.014 Uiso 1 1 calc R U .
C7 C 0.2401(2) 0.70800(15) 0.39873(15) 0.0121(3) Uani 1 1 d . . .
C8 C 0.2135(2) 0.22382(15) 0.34758(14) 0.0100(3) Uani 1 1 d . . .
C9 C 0.3507(2) 0.39233(15) 0.76662(14) 0.0102(3) Uani 1 1 d . . .
C10 C -0.0761(2) -0.07089(17) 0.08857(15) 0.0142(3) Uani 1 1 d . . .
H10 H -0.133267 -0.122227 0.149437 0.017 Uiso 1 1 calc R U .
C11 C 0.1516(2) 0.04706(17) 0.02821(15) 0.0142(3) Uani 1 1 d . . .
H11 H 0.260023 0.081521 0.045062 0.017 Uiso 1 1 calc R U .
N1 N 0.07548(19) -0.02335(13) 0.11778(12) 0.0117(3) Uani 1 1 d . . .
O1 O 0.21120(18) 0.72978(11) 0.28373(11) 0.0165(2) Uani 1 1 d . . .
O2 O 0.25643(18) 0.80287(12) 0.46714(12) 0.0179(3) Uani 1 1 d . . .
O3 O 0.19777(17) 0.24689(12) 0.23329(11) 0.0156(2) Uani 1 1 d . . .
O4 O 0.20465(17) 0.11032(11) 0.40001(11) 0.0145(2) Uani 1 1 d . . .
O5 O 0.35895(17) 0.27689(11) 0.81323(11) 0.0145(2) Uani 1 1 d . . .
O6 O 0.37572(17) 0.49275(11) 0.82660(11) 0.0144(2) Uani 1 1 d . . .
O7 O 0.43794(18) -0.04894(14) 0.23082(13) 0.0177(3) Uani 1 1 d . . .
O8 O -0.07192(18) -0.05985(14) 0.36744(13) 0.0160(2) Uani 1 1 d . . .
O9 O 0.74227(19) 0.41011(14) 0.92563(13) 0.0189(3) Uani 1 1 d . . .
O10 O 0.44111(19) 0.31196(13) 1.05360(13) 0.0169(3) Uani 1 1 d . . .
O11 O 0.1474(2) 0.71955(15) 0.85320(13) 0.0247(3) Uani 1 1 d . . .
O12 O 0.6538(2) 0.12803(14) 0.30189(15) 0.0235(3) Uani 1 1 d . . .
Co1 Co 0.500000 0.500000 1.000000 0.00888(8) Uani 1 2 d S . P
Zn1 Zn 0.18666(3) -0.05664(2) 0.30260(2) 0.01242(7) Uani 1 1 d . . .
H7A H 0.493(4) 0.000(3) 0.254(2) 0.026(7) Uiso 1 1 d . . .
H7B H 0.499(3) -0.116(3) 0.225(2) 0.025(6) Uiso 1 1 d . . .
H8A H -0.143(4) -0.005(3) 0.348(2) 0.021(6) Uiso 1 1 d . . .
H8B H -0.086(4) -0.078(3) 0.429(3) 0.026(7) Uiso 1 1 d . . .
H9A H 0.743(3) 0.377(3) 0.863(3) 0.029(7) Uiso 1 1 d . . .
H9B H 0.786(4) 0.370(3) 0.977(3) 0.034(8) Uiso 1 1 d . . .
H10A H 0.404(4) 0.291(3) 0.998(3) 0.039(8) Uiso 1 1 d . . .
H10B H 0.370(4) 0.304(3) 1.107(3) 0.032(7) Uiso 1 1 d . . .
H11A H 0.043(5) 0.723(3) 0.826(3) 0.052(9) Uiso 1 1 d . . .
H11B H 0.206(4) 0.643(3) 0.833(3) 0.046(8) Uiso 1 1 d . . .
H12A H 0.662(4) 0.159(3) 0.368(3) 0.038(8) Uiso 1 1 d . . .
H12B H 0.697(4) 0.173(3) 0.249(3) 0.040(8) Uiso 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'
Co Co 0.3494 0.9721 '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'
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
C6 C1 C2 119.33(14) . .
C6 C1 C7 119.72(14) . .
C2 C1 C7 120.95(14) . .
C3 C2 C1 120.37(14) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C4 C3 C2 119.66(14) . .
C4 C3 C8 121.34(14) . .
C2 C3 C8 119.00(14) . .
C5 C4 C3 120.36(14) . .
C5 C4 H4 119.8 . .
C3 C4 H4 119.8 . .
C6 C5 C4 119.35(14) . .
C6 C5 C9 120.01(13) . .
C4 C5 C9 120.63(14) . .
C1 C6 C5 120.91(14) . .
C1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
O2 C7 O1 119.79(15) . .
O2 C7 C1 120.45(14) . .
O1 C7 C1 119.76(14) . .
O2 C7 Zn1 61.73(8) . 1_565
O1 C7 Zn1 58.27(8) . 1_565
C1 C7 Zn1 174.55(12) . 1_565
O3 C8 O4 123.52(14) . .
O3 C8 C3 119.06(14) . .
O4 C8 C3 117.41(13) . .
O5 C9 O6 124.39(14) . .
O5 C9 C5 119.28(14) . .
O6 C9 C5 116.33(14) . .
N1 C10 C11 121.68(15) . 2
N1 C10 H10 119.2 . .
C11 C10 H10 119.2 2 .
N1 C11 C10 121.57(15) . 2
N1 C11 H11 119.2 . .
C10 C11 H11 119.2 2 .
C11 N1 C10 116.74(14) . .
C11 N1 Zn1 122.20(11) . .
C10 N1 Zn1 121.05(11) . .
C7 O1 Zn1 92.19(10) . 1_565
C7 O2 Zn1 88.88(10) . 1_565
C8 O4 Zn1 123.18(10) . .
C9 O6 Co1 128.62(10) . .
Zn1 O7 H7A 119(2) . .
Zn1 O7 H7B 117.4(19) . .
H7A O7 H7B 108(3) . .
Zn1 O8 H8A 120.0(19) . .
Zn1 O8 H8B 119(2) . .
H8A O8 H8B 109(3) . .
Co1 O9 H9A 120(2) . .
Co1 O9 H9B 106(2) . .
H9A O9 H9B 116(3) . .
Co1 O10 H10A 102(2) . .
Co1 O10 H10B 119(2) . .
H10A O10 H10B 106(3) . .
H11A O11 H11B 107(3) . .
H12A O12 H12B 109(3) . .
O10 Co1 O10 180.0 . 2_667
O10 Co1 O9 87.60(6) . .
O10 Co1 O9 92.40(6) 2_667 .
O10 Co1 O9 92.40(6) . 2_667
O10 Co1 O9 87.60(6) 2_667 2_667
O9 Co1 O9 180.0 . 2_667
O10 Co1 O6 91.90(5) . .
O10 Co1 O6 88.10(5) 2_667 .
O9 Co1 O6 90.55(5) . .
O9 Co1 O6 89.45(5) 2_667 .
O10 Co1 O6 88.10(5) . 2_667
O10 Co1 O6 91.90(5) 2_667 2_667
O9 Co1 O6 89.45(5) . 2_667
O9 Co1 O6 90.55(5) 2_667 2_667
O6 Co1 O6 180.0 . 2_667
O7 Zn1 O4 90.68(5) . .
O7 Zn1 O8 177.27(6) . .
O4 Zn1 O8 89.63(5) . .
O7 Zn1 N1 90.42(5) . .
O4 Zn1 N1 115.60(5) . .
O8 Zn1 N1 87.00(5) . .
O7 Zn1 O1 91.20(5) . 1_545
O4 Zn1 O1 153.18(5) . 1_545
O8 Zn1 O1 89.74(5) . 1_545
N1 Zn1 O1 91.14(5) . 1_545
O7 Zn1 O2 98.67(5) . 1_545
O4 Zn1 O2 94.43(5) . 1_545
O8 Zn1 O2 84.01(5) . 1_545
N1 Zn1 O2 148.57(5) . 1_545
O1 Zn1 O2 58.85(4) 1_545 1_545
O7 Zn1 C7 97.15(5) . 1_545
O4 Zn1 C7 123.82(5) . 1_545
O8 Zn1 C7 84.93(5) . 1_545
N1 Zn1 C7 119.85(5) . 1_545
O1 Zn1 C7 29.53(5) 1_545 1_545
O2 Zn1 C7 29.39(5) 1_545 1_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C6 1.391(2) .
C1 C2 1.395(2) .
C1 C7 1.498(2) .
C2 C3 1.395(2) .
C2 H2 0.9500 .
C3 C4 1.394(2) .
C3 C8 1.507(2) .
C4 C5 1.394(2) .
C4 H4 0.9500 .
C5 C6 1.392(2) .
C5 C9 1.507(2) .
C6 H6 0.9500 .
C7 O2 1.257(2) .
C7 O1 1.264(2) .
C7 Zn1 2.5614(16) 1_565
C8 O3 1.2449(19) .
C8 O4 1.2739(19) .
C9 O5 1.2544(19) .
C9 O6 1.2661(19) .
C10 N1 1.340(2) .
C10 C11 1.386(2) 2
C10 H10 0.9500 .
C11 N1 1.339(2) .
C11 H11 0.9500 .
N1 Zn1 2.1656(14) .
O1 Zn1 2.1803(12) 1_565
O2 Zn1 2.2563(12) 1_565
O4 Zn1 2.0533(11) .
O6 Co1 2.1066(11) .
O7 Zn1 2.0419(13) .
O7 H7A 0.74(3) .
O7 H7B 0.79(3) .
O8 Zn1 2.0623(13) .
O8 H8A 0.75(3) .
O8 H8B 0.69(3) .
O9 Co1 2.1037(13) .
O9 H9A 0.76(3) .
O9 H9B 0.73(3) .
O10 Co1 2.0746(13) .
O10 H10A 0.71(3) .
O10 H10B 0.79(3) .
O11 H11A 0.84(4) .
O11 H11B 0.89(3) .
O12 H12A 0.79(3) .
O12 H12B 0.80(3) .
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
_geom_hbond_publ_flag
C10 H10 O5 0.95 2.47 3.297(2) 145.5 2_556 yes
C10 H10 O8 0.95 2.52 3.002(2) 111.9 . yes
C11 H11 O7 0.95 2.64 3.135(2) 112.7 . yes
O7 H7A O12 0.74(3) 1.97(3) 2.709(2) 174(3) . yes
O7 H7B O5 0.79(3) 1.90(3) 2.6808(18) 173(3) 2_656 yes
O8 H8A O12 0.75(3) 1.98(3) 2.726(2) 175(3) 1_455 yes
O8 H8B O4 0.69(3) 2.06(3) 2.7264(18) 163(3) 2_556 yes
O9 H9A O1 0.76(3) 1.96(3) 2.7077(18) 168(3) 2_666 yes
O9 H9B O11 0.73(3) 2.05(3) 2.761(2) 165(3) 2_667 yes
O10 H10A O5 0.71(3) 2.03(3) 2.7126(18) 160(3) . yes
O10 H10B O3 0.79(3) 1.98(3) 2.7553(18) 169(3) 1_556 yes
O11 H11A O3 0.84(4) 1.92(4) 2.756(2) 173(3) 2_566 yes
O11 H11B O6 0.89(3) 1.88(3) 2.7348(19) 163(3) . yes
O12 H12A O2 0.79(3) 1.96(3) 2.7244(19) 163(3) 2_666 yes
O12 H12B O11 0.80(3) 1.98(3) 2.773(2) 166(3) 2_666 yes
