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#$Date: 2022-03-22 12:22:33 +0200 (Tue, 22 Mar 2022) $
#$Revision: 273894 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/48/8104831.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_8104831
loop_
_publ_author_name
'Lan, Ying-Dong'
'Xiong, Chun-Lan'
'Huang, Cui-xin'
'Xiong, Wan-Ming'
'Nie, Xu-Liang'
_publ_section_title
;
 Crystal structure of tetraaqua-bis(1H-indazole-6-carboxylate-\kN)cadmium
 (II), C16H18CdN4O8
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              359
_journal_page_last               361
_journal_paper_doi               10.1515/ncrs-2020-0581
_journal_volume                  236
_journal_year                    2021
_chemical_formula_sum            'C16 H18 Cd N4 O8'
_chemical_formula_weight         506.74
_chemical_name_systematic
;bis-(1H-indazole-6-carboxylate-k N²)-
cadmium (II), tetrahydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90.7930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2751(4)
_cell_length_b                   21.7902(13)
_cell_length_c                   13.3401(8)
_cell_measurement_reflns_used    7748
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.45
_cell_volume                     1823.89(19)
_computing_cell_refinement       'APEX2, SAINT and SADABS [1]'
_computing_data_collection       'APEX2, SAINT and SADABS [1]'
_computing_data_reduction        'APEX2, SAINT and SADABS [1]'
_computing_molecular_graphics    'Diamond 4.0 [4]'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014) [2,3]'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014) [2,3]'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014) [2,3]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13899
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.414
_exptl_absorpt_coefficient_mu    1.253
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Crystallogr. B69 (2013) 249-259).
;
_refine_ls_extinction_coef       0.00052(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0226P)²+1.8787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3074
_reflns_number_total             3398
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0581_suppl.cif
_cod_data_source_block           3349_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8104831
_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   0.952
_shelx_estimated_absorpt_t_max   0.963
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.73109(3) 0.24657(2) 0.12363(2) 0.02646(8) Uani 1 1 d . . . . .
N1 N 0.8087(4) 0.35180(10) 0.12669(17) 0.0338(5) Uani 1 1 d . . . . .
N2 N 0.6853(4) 0.39968(10) 0.09396(18) 0.0333(5) Uani 1 1 d . . . . .
N3 N 0.6574(4) 0.14095(10) 0.13023(18) 0.0336(5) Uani 1 1 d . . . . .
N4 N 0.7913(4) 0.09632(10) 0.09807(18) 0.0297(5) Uani 1 1 d . . . . .
O1 O 0.9209(3) 0.66753(8) 0.12391(15) 0.0399(5) Uani 1 1 d . . . . .
O2 O 0.6622(3) 0.63481(8) 0.02220(17) 0.0472(6) Uani 1 1 d . . . . .
O3 O 0.9044(3) -0.13461(8) 0.03350(18) 0.0492(6) Uani 1 1 d . . . . .
O4 O 0.6169(4) -0.17608(9) 0.09721(17) 0.0498(6) Uani 1 1 d . . . . .
O5 O 0.8819(3) 0.23963(10) -0.03148(16) 0.0346(4) Uani 1 1 d . . . . .
O6 O 1.0618(4) 0.22785(13) 0.1927(2) 0.0492(6) Uani 1 1 d . . . . .
O7 O 0.6059(5) 0.24982(13) 0.28438(19) 0.0544(7) Uani 1 1 d . . . . .
O8 O 0.3944(3) 0.25607(10) 0.05675(16) 0.0301(4) Uani 1 1 d . . . . .
C1 C 0.9888(4) 0.37567(12) 0.1608(2) 0.0342(6) Uani 1 1 d . . . . .
H1 H 1.1003 0.3529 0.1886 0.041 Uiso 1 1 calc R U . . .
C2 C 0.9906(4) 0.43998(11) 0.14981(18) 0.0268(5) Uani 1 1 d . . . . .
C3 C 0.7909(4) 0.45379(11) 0.10648(18) 0.0269(5) Uani 1 1 d . . . . .
C4 C 0.7283(4) 0.51408(11) 0.0851(2) 0.0297(6) Uani 1 1 d . . . . .
H4A H 0.5951 0.5226 0.0570 0.036 Uiso 1 1 calc R U . . .
C5 C 0.8707(4) 0.56011(11) 0.10696(18) 0.0276(5) Uani 1 1 d . . . . .
C6 C 1.0736(4) 0.54699(12) 0.14965(19) 0.0296(6) Uani 1 1 d . . . . .
H6 H 1.1670 0.5791 0.1638 0.036 Uiso 1 1 calc R U . . .
C7 C 1.1351(4) 0.48783(12) 0.17056(19) 0.0294(6) Uani 1 1 d . . . . .
H7 H 1.2692 0.4796 0.1978 0.035 Uiso 1 1 calc R U . . .
C8 C 0.8135(4) 0.62551(11) 0.0834(2) 0.0314(6) Uani 1 1 d . . . . .
C9 C 0.4838(4) 0.11286(12) 0.1622(2) 0.0343(6) Uani 1 1 d . . . . .
H9 H 0.3671 0.1327 0.1896 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4997(4) 0.04887(11) 0.14921(18) 0.0257(5) Uani 1 1 d . . . . .
C11 C 0.7010(4) 0.04017(11) 0.10771(18) 0.0237(5) Uani 1 1 d . . . . .
C12 C 0.7794(4) -0.01819(11) 0.08512(19) 0.0263(5) Uani 1 1 d . . . . .
H12 H 0.9152 -0.0234 0.0594 0.032 Uiso 1 1 calc R U . . .
C13 C 0.6492(4) -0.06750(11) 0.10217(18) 0.0253(5) Uani 1 1 d . . . . .
C14 C 0.4427(4) -0.05936(12) 0.14292(19) 0.0285(6) Uani 1 1 d . . . . .
H14 H 0.3570 -0.0935 0.1535 0.034 Uiso 1 1 calc R U . . .
C15 C 0.3679(4) -0.00250(12) 0.16674(19) 0.0286(5) Uani 1 1 d . . . . .
H15 H 0.2333 0.0024 0.1939 0.034 Uiso 1 1 calc R U . . .
C16 C 0.7292(4) -0.13051(12) 0.0763(2) 0.0323(6) Uani 1 1 d . . . . .
H1W H 0.953(5) 0.2664(15) -0.049(2) 0.032(9) Uiso 1 1 d . . . . .
H2W H 0.956(6) 0.208(2) -0.035(3) 0.081(15) Uiso 1 1 d . . . . .
H3W H 1.154(7) 0.2324(19) 0.167(3) 0.063(15) Uiso 1 1 d . . . . .
H4W H 1.073(5) 0.2108(15) 0.242(3) 0.038(10) Uiso 1 1 d . . . . .
H5W H 0.676(9) 0.244(2) 0.328(5) 0.12(2) Uiso 1 1 d . . . . .
H6W H 0.525(7) 0.2713(19) 0.306(3) 0.066(14) Uiso 1 1 d . . . . .
H7W H 0.374(5) 0.2880(18) 0.034(3) 0.054(11) Uiso 1 1 d . . . . .
H8W H 0.387(5) 0.2320(16) 0.009(3) 0.045(10) Uiso 1 1 d . . . . .
H2 H 0.567(4) 0.3903(13) 0.063(2) 0.032(8) Uiso 1 1 d . . . . .
H4 H 0.899(5) 0.1054(13) 0.067(2) 0.032(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'
Cd Cd -0.8075 1.2024 '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
O8 Cd1 O5 92.55(8) . .
O8 Cd1 O7 92.02(10) . .
O5 Cd1 O7 175.15(9) . .
O8 Cd1 O6 174.84(9) . .
O5 Cd1 O6 88.17(9) . .
O7 Cd1 O6 87.13(11) . .
O8 Cd1 N1 96.24(8) . .
O5 Cd1 N1 89.54(8) . .
O7 Cd1 N1 91.57(9) . .
O6 Cd1 N1 88.87(9) . .
O8 Cd1 N3 85.54(8) . .
O5 Cd1 N3 93.04(8) . .
O7 Cd1 N3 85.70(9) . .
O6 Cd1 N3 89.32(9) . .
N1 Cd1 N3 176.80(8) . .
C1 N1 N2 106.7(2) . .
C1 N1 Cd1 124.63(17) . .
N2 N1 Cd1 128.62(17) . .
C3 N2 N1 110.4(2) . .
C3 N2 H2 132.3(18) . .
N1 N2 H2 116.7(18) . .
C9 N3 N4 106.6(2) . .
C9 N3 Cd1 128.87(17) . .
N4 N3 Cd1 124.51(17) . .
C11 N4 N3 110.8(2) . .
C11 N4 H4 128(2) . .
N3 N4 H4 120(2) . .
Cd1 O5 H1W 118(2) . .
Cd1 O5 H2W 110(3) . .
H1W O5 H2W 107(4) . .
Cd1 O6 H3W 122(4) . .
Cd1 O6 H4W 121(2) . .
H3W O6 H4W 116(4) . .
Cd1 O7 H5W 122(5) . .
Cd1 O7 H6W 128(3) . .
H5W O7 H6W 102(5) . .
Cd1 O8 H7W 112(3) . .
Cd1 O8 H8W 107(2) . .
H7W O8 H8W 105(3) . .
N1 C1 C2 111.4(2) . .
N1 C1 H1 124.3 . .
C2 C1 H1 124.3 . .
C3 C2 C7 119.4(2) . .
C3 C2 C1 104.3(2) . .
C7 C2 C1 136.3(2) . .
N2 C3 C4 130.8(2) . .
N2 C3 C2 107.1(2) . .
C4 C3 C2 122.1(2) . .
C5 C4 C3 117.5(2) . .
C5 C4 H4A 121.2 . .
C3 C4 H4A 121.2 . .
C4 C5 C6 121.1(2) . .
C4 C5 C8 119.7(2) . .
C6 C5 C8 119.1(2) . .
C7 C6 C5 121.3(2) . .
C7 C6 H6 119.3 . .
C5 C6 H6 119.3 . .
C6 C7 C2 118.5(2) . .
C6 C7 H7 120.7 . .
C2 C7 H7 120.7 . .
O1 C8 O2 123.9(2) . .
O1 C8 C5 118.5(2) . .
O2 C8 C5 117.7(2) . .
N3 C9 C10 111.0(2) . .
N3 C9 H9 124.5 . .
C10 C9 H9 124.5 . .
C11 C10 C9 104.4(2) . .
C11 C10 C15 119.5(2) . .
C9 C10 C15 136.2(2) . .
N4 C11 C12 130.7(2) . .
N4 C11 C10 107.2(2) . .
C12 C11 C10 122.1(2) . .
C13 C12 C11 117.7(2) . .
C13 C12 H12 121.2 . .
C11 C12 H12 121.2 . .
C12 C13 C14 120.9(2) . .
C12 C13 C16 118.4(2) . .
C14 C13 C16 120.7(2) . .
C15 C14 C13 121.3(2) . .
C15 C14 H14 119.3 . .
C13 C14 H14 119.3 . .
C14 C15 C10 118.5(2) . .
C14 C15 H15 120.7 . .
C10 C15 H15 120.7 . .
O3 C16 O4 123.2(3) . .
O3 C16 C13 118.0(2) . .
O4 C16 C13 118.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O8 2.2911(19) .
Cd1 O5 2.292(2) .
Cd1 O7 2.295(2) .
Cd1 O6 2.295(2) .
Cd1 N1 2.344(2) .
Cd1 N3 2.349(2) .
N1 C1 1.319(3) .
N1 N2 1.367(3) .
N2 C3 1.362(3) .
N2 H2 0.87(3) .
N3 C9 1.325(3) .
N3 N4 1.359(3) .
N4 C11 1.355(3) .
N4 H4 0.82(3) .
O1 C8 1.255(3) .
O2 C8 1.260(3) .
O3 C16 1.249(3) .
O4 C16 1.251(3) .
O5 H1W 0.77(3) .
O5 H2W 0.84(4) .
O6 H3W 0.69(4) .
O6 H4W 0.76(4) .
O7 H5W 0.73(6) .
O7 H6W 0.75(4) .
O8 H7W 0.77(4) .
O8 H8W 0.83(4) .
C1 C2 1.409(4) .
C1 H1 0.9300 .
C2 C3 1.405(3) .
C2 C7 1.407(3) .
C3 C4 1.400(4) .
C4 C5 1.372(3) .
C4 H4A 0.9300 .
C5 C6 1.417(4) .
C5 C8 1.502(3) .
C6 C7 1.373(4) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C9 C10 1.409(4) .
C9 H9 0.9300 .
C10 C11 1.399(3) .
C10 C15 1.413(3) .
C11 C12 1.398(3) .
C12 C13 1.371(3) .
C12 H12 0.9300 .
C13 C14 1.423(3) .
C13 C16 1.504(3) .
C14 C15 1.364(4) .
C14 H14 0.9300 .
C15 H15 0.9300 .
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 H4 O3 0.82(3) 1.94(3) 2.741(3) 164(3) 3_755
N2 H2 O2 0.87(3) 1.90(3) 2.762(3) 171(3) 3_665
O8 H8W O4 0.83(4) 1.86(4) 2.694(3) 177(3) 3_655
O8 H7W O2 0.77(4) 1.85(4) 2.623(3) 178(4) 3_665
O7 H6W O4 0.75(4) 1.95(4) 2.668(3) 159(4) 2_655
O7 H5W O5 0.73(6) 2.29(6) 2.995(4) 162(6) 4_566
O6 H4W O1 0.76(4) 2.02(4) 2.778(3) 175(3) 2_745
O6 H3W O8 0.69(4) 2.18(5) 2.851(4) 166(5) 1_655
O5 H2W O3 0.84(4) 1.82(4) 2.652(3) 174(4) 3_755
O5 H1W O1 0.77(3) 1.93(3) 2.681(3) 165(3) 3_765
