Coordination chemistry of flexible benzene-1,3,5-tricarboxamide derived carboxylates; notable structural resilience and vaguely familiar packing motifs.
Lynes, Amy D.; Hawes, Chris S.; Byrne, Kevin; Schmitt, Wolfgang; Gunnlaugsson, Thorfinnur; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5259–5268; doi:10.1039/C8DT00439K

data_7045846
_publ_section_title
;
 Coordination chemistry of flexible benzene-1,3,5-tricarboxamide derived
 carboxylates; notable structural resilience and vaguely familiar packing
 motifs.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5259
_journal_page_last               5268
_journal_paper_doi               10.1039/C8DT00439K
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C33 H37 Cd3 N7 O22, 5(H2 O)'
_chemical_formula_sum            'C33 H47 Cd3 N7 O27'
_chemical_formula_weight         1310.97
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-21 deposited with the CCDC.
2018-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.6750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0689(6)
_cell_length_b                   22.3544(9)
_cell_length_c                   14.3047(6)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.49
_cell_volume                     4537.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            132473
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         1.435
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0693 before and 0.0503 after correction. The Ratio of minimum to maximum transmission is 0.8421. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.618
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         11504
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+15.0890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10328
_reflns_number_total             11504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00439k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7045845--7045847.cif.'
_cod_database_code               7045846
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H22A-O7
 1.9 with sigma of 0.02
 H22B-O28
 1.9 with sigma of 0.02
 H29C-O28
 2.25 with sigma of 0.02
 H26D-O24
 2 with sigma of 0.02
 H23B-O3
 2.131 with sigma of 0.001
 H23A-O12_$1
 2 with sigma of 0.001
 H21B-O4_$1
 1.88 with sigma of 0.01
 H21A-O19_$4
 1.88 with sigma of 0.01
 H27A-O25
 2 with sigma of 0.02
 H25A-O13_$2
 1.981 with sigma of 0.001
 H25B-O23
 3.141 with sigma of 0.001
 H20A_$3-H25B
 2.15 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.05
4. Others
 Fixed Sof: O24(0.75) H24A(0.75) H24B(0.75) O25(0.25) H25A(0.25) H25B(0.25)
 O26(0.6667) H26C(0.6667) H26D(0.6667) O27(0.33333) H27A(0.33333) H27B(0.33333)
5.a Free rotating group:
 O29(H29C,H29D), O23(H23A,H23B), O24(H24A,H24B), O25(H25A,H25B), O26(H26C,
 H26D), O27(H27A,H27B), O28(H28A,H28B)
5.b Rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O22(H22A,H22B)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C11(H11A,H11B), C14(H14A,H14B), C17(H17A,H17B), C26(H26A,H26B),
 C29(H29A,H29B)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C5(H5A), C7(H7), C9(H9),
 C20(H20), C22(H22), C24(H24), C31(H31)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              90282
_olex2_submission_special_instructions 'No special instructions were received'