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_7045847
_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
'C72 H60 Cd3 N8 O19.85, 2(H2 O), 0.5(O), 2.35(C3 H7 N O)'
_chemical_formula_sum            'C79.05 H81.45 Cd3 N10.35 O24.7'
_chemical_formula_weight         1908.89
_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
_atom_sites_solution_primary     direct
_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                101.9120(10)
_cell_angle_beta                 101.2140(10)
_cell_angle_gamma                98.7420(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3062(3)
_cell_length_b                   20.1158(6)
_cell_length_c                   22.2589(7)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.26
_cell_volume                     3918.4(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.058
_diffrn_reflns_theta_min         1.592
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.4293
_exptl_absorpt_correction_T_min  0.3740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0551 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.8712. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.239
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         15470
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      8.294
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+8.4869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10666
_reflns_number_total             15470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00439k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7045845--7045847.cif.'
_cod_original_formula_sum        'C79.05 H81.45 Cd3 N10.35 O24.70'
_cod_database_code               7045847
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.807
_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
 Cd3A_$2-O8A
 2.2 with sigma of 0.01
 O8A-C33 = O8-C33
 1.3 with sigma of 0.01
 O17-C66
 1.25 with sigma of 0.01
 C66-C65
 1.5 with sigma of 0.01
 O18-C66
 1.3 with sigma of 0.01
 O18A-Cd2A_$2
 2.2 with sigma of 0.01
 O18A-C66
 1.255 with sigma of 0.01
 C77-C76
 2.45 with sigma of 0.02
 H24B-O23
 1.879 with sigma of 0.01
 C78-C77
 2.45 with sigma of 0.01
 C78-C76
 2.45 with sigma of 0.01
 O10A-C34 \\sim O10-C34 \\sim O11-C34 \\sim O11A-C34
 with sigma of 0.02
 Cd2A-O10A \\sim Cd2-O10
 with sigma of 0.02
 Cd1_$3-O8A \\sim Cd1_$3-O8
 with sigma of 0.01
 N10-C77 \\sim N10-C78
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O18) \\sim Ueq, Uanis(O18A) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
Uanis(O10) = Uanis(O10A)
Uanis(O8A) = Uanis(O8)
Uanis(O18) = Uanis(O18A)
Uanis(C77) = Uanis(C78)
4. Others
 Fixed Sof: Cd2(0.85) Cd2A(0.15) Cd3(0.85) Cd3A(0.15) O8(0.85) O10(0.85)
 O10A(0.15) O11(0.85) O11A(0.15) O17(0.85) O18(0.85) O25(0.5) O20(0.85)
 N8(0.85) C70(0.85) H70(0.85) C71(0.85) H71A(0.85) H71B(0.85) H71C(0.85)
 C72(0.85) H72A(0.85) H72B(0.85) H72C(0.85) O22(0.5) N10(0.5) C76(0.5) H76(0.5)
 C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C78(0.5) H78A(0.5) H78B(0.5) H78C(0.5)
 O8A(0.15) O18A(0.15)
5.a Free rotating group:
 O23(H23C,H23D), O24(H24A,H24B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C23(H23A,H23B), C35(H35A,H35B), C56(H56A,H56B), C65(H65A,H65B)
5.c Me refined with riding coordinates:
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,
 H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C4(H4A), C5(H5A), C7(H7),
 C8(H8), C11(H11), C13(H13), C15(H15), C18(H18), C19(H19), C21(H21), C22(H22),
 C27(H27), C28(H28), C30(H30), C31(H31), C37(H37), C38(H38), C40(H40), C41(H41),
  C44(H44), C46(H46), C48(H48), C51(H51), C52(H52), C54(H54), C55(H55),
 C60(H60), C61(H61), C63(H63), C64(H64), C67(H67), C79(H79), C70(H70), C73(H73),
  C76(H76)
;
_shelx_res_checksum              10853
_olex2_submission_special_instructions 'No special instructions were received'