Crystal structure of catena-poly[(5,5′-dimethyl-2,2′-bipyridine-κ 2 N,N′)-(μ 3-hydrogen-1,1′,1″-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylato)- κ 5 O:O,O′:O″,O‴)-cadmium(II)], C33H40CdN8O6
Zhang, Hua-Xiang; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 1051–1053; doi:10.1515/ncrs-2022-0351

data_8107291
_publ_section_title
;
 Crystal structure of
 catena-poly[(5,5&#x2032;-dimethyl-2,2&#x2032;-bipyridine-\k 2
 N,N&#x2032;)-(\m
 3-hydrogen-1,1&#x2032;,1&#x2033;-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylato)-
 \k 5 O:O,O&#x2032;:O&#x2033;,O&#x2034;)-cadmium(II)], C33H40CdN8O6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1051
_journal_page_last               1053
_journal_paper_doi               10.1515/ncrs-2022-0351
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C33 H40 Cd N8 O6'
_chemical_formula_sum            'C33 H40 Cd N8 O6'
_chemical_formula_weight         757.13
_chemical_name_systematic
;
catena-[(5,5'-dimethyl-2,2'-bipyridine-\k^2^ N, N')-(\m~3~-hydrogen 
1,1',1''-(1,3,5-triazine-2,4,6-triyl)tris(piperidine-4-carboxylato)-\k^6^ 
O, O, O', O'', O''')-cadmium(II)]
;
_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     dual
_cell_angle_alpha                93.976(5)
_cell_angle_beta                 102.005(7)
_cell_angle_gamma                111.827(8)
_cell_formula_units_Z            2
_cell_length_a                   10.6468(11)
_cell_length_b                   11.6739(9)
_cell_length_c                   14.5312(9)
_cell_measurement_reflns_used    2281
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.9320
_cell_measurement_theta_min      3.1290
_cell_volume                     1618.4(3)
_computing_cell_refinement       'SAINT v6.02A (Bruker, 2001) [1]'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.02A (Bruker, 2001) [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015) [3]'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015) [4]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2563
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Advance CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10151
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         5699
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0480
_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^+0.1928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4293
_reflns_number_total             5699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0351_suppl.cif
_cod_data_source_block           exp_2927
_cod_original_cell_volume        1618.4(2)
_cod_database_code               8107291
_chemical_oxdiff_formula         C10H11O2S
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2_$1-H2_$1
 0.82 with sigma of 0.02
3. Rigid bond restraints
 Cd1, O5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim O2 \\sim O1A \\sim O1: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 3.8A
5. Others
 Sof(O1A)=1-FVAR(1)
 Sof(O1)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C2(H2a), C11(H11), C18(H18)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b), C9(H9a,H9b), C10(H10a,
 H10b), C13(H13a,H13b), C14(H14a,H14b), C16(H16a,H16b), C17(H17a,H17b),
 C19(H19a,H19b), C20(H20a,H20b)
6.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C24(H24), C25(H25), C28(H28), C29(H29), C31(H31)
6.d Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c)
;
_olex2_submission_special_instructions 'No special instructions were received'