The crystal structure of poly[(μ2-terephthalato-κ4 O,O′: O″,O‴)-(μ4-terephthalato-κ4 O:O′:O″:O‴)-{μ4-(1,2,4,5-tetrakis(1,2,4-triazol-1-ylmethyl)-benzene-κ4 O:O′:O″,O‴)}dicadmium(II)] – water – acetronitrile (1/2/2), C38H36N14O10Cd2
Wang, Hua-Rui; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 389–391; doi:10.1515/ncrs-2022-0053

data_8105704
_publ_section_title
;
 The crystal structure of poly[(\m2-terephthalato-\k4 O,O&#x2032;:
 O&#x2033;,O&#x2034;)-(\m4-terephthalato-\k4
 O:O&#x2032;:O&#x2033;:O&#x2034;)-{\m4-(1,2,4,5-tetrakis(1,2,4-triazol-1-ylmethyl)-benzene-\k4
 O:O&#x2032;:O&#x2033;,O&#x2034;)}dicadmium(II)]&#x00A0;-- water&#x00A0;--
 acetronitrile (1/2/2), C38H36N14O10Cd2
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              389
_journal_page_last               391
_journal_paper_doi               10.1515/ncrs-2022-0053
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C34 H26 Cd2 N12 O8, 2(H2 O), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H36 Cd2 N14 O10'
_chemical_formula_weight         1073.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                84.18(3)
_cell_angle_beta                 72.02(3)
_cell_angle_gamma                75.28(3)
_cell_formula_units_Z            1
_cell_length_a                   10.220(2)
_cell_length_b                   10.685(2)
_cell_length_c                   10.777(2)
_cell_measurement_reflns_used    4003
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8764
_cell_measurement_theta_min      1.9872
_cell_volume                     1082.3(4)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13220
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         2.764
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0268
_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/[\s^2^(Fo^2^)+(0.0354P)^2^+0.9668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4850
_reflns_number_total             5081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0053_suppl.cif
_cod_data_source_block           a
_cod_database_code               8105704
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C5-C4 = C19-C1
 1.45 with sigma of 0.02
 N8-C5 = N4-C1
 1.2 with sigma of 0.02
 N4A-N5A \\sim N6A-C18A
 with sigma of 0.02
 N4A-N5A \\sim C18A-N6A
 with sigma of 0.02
 N6A-N4A \\sim N5A-C7A
 with sigma of 0.02
 N4A-C7A \\sim N6A-C7A \\sim N6A-N5A \\sim N5A-C18A \\sim N4A-C18A \\sim N7-C18
\\sim N5-C18 \\sim N6-N5 ~
 N6-C7 \\sim N7-C7
 with sigma of 0.02
3. Rigid bond restraints
 C5, N8, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N4A) = Uanis(C18) = Uanis(C18A)
Uanis(N5) = Uanis(N5A)
Uanis(N6) = Uanis(N6A)
Uanis(N4A) = Uanis(N7)
Uanis(C7A) = Uanis(C7)
Uanis(N4) = Uanis(N8)
Uanis(C1) = Uanis(C5)
Uanis(C19) = Uanis(C4)
5. Others
 Sof(H14C)=Sof(H14D)=Sof(N4A)=Sof(N5A)=Sof(N6A)=Sof(C7A)=Sof(H7A)=Sof(C18A)=
 Sof(H18A)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(N5)=Sof(N6)=Sof(N7)=Sof(C7)=Sof(H7)=Sof(C18)=Sof(H18)=
 FVAR(1)
 Sof(N8)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=1-FVAR(2)
 Sof(N4)=Sof(C1)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
6.a Riding coordinates:
 O6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C14(H14C,H14D), C22(H22A,H22B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C13(H13), C15(H15), C16(H16), C24(H24), C25(H25), C7(H7),
 C18(H18), C7A(H7A), C18A(H18A)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              50539
_shelx_hkl_checksum              64640
_olex2_submission_special_instructions 'No special instructions were received'