A folded [2× 2] metallo-supramolecular grid from a bis-tridentate (1,2,3-triazol-4-yl)-picolinamide (tzpa) ligand
Barry, Dawn; Hawes, Chris Samuel; Byrne, Joseph Peter; la Cour Poulsen, Bjørn; Ruether, Manuel; O'Brien, John E; Gunnlaugsson, Thorfinnur; Dalton Trans.  (2017) –; doi:10.1039/C7DT01533J

data_7042832
_publ_section_title
;
 A folded [2\\times 2] metallo-supramolecular grid from a bis-tridentate
 (1,2,3-triazol-4-yl)-picolinamide (tzpa) ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01533J
_journal_year                    2017
_chemical_formula_moiety         'C168 H144 N40 O24 Zn4, 8(Cl O4), 8(C2 H3 N)'
_chemical_formula_sum            'C184 H168 Cl8 N48 O56 Zn4'
_chemical_formula_weight         4492.73
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8871(8)
_cell_length_b                   24.8871(8)
_cell_length_c                   34.3819(14)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.97
_cell_measurement_theta_min      2.19
_cell_volume                     21295.0(13)
_computing_cell_refinement       'SAINT V8.35A (2016)'
_computing_data_reduction        'SAINT V8.35A (2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            84206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.513
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0894 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.8195. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             9248
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0904P)^2^+28.8792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7952
_reflns_number_total             9768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01533j2.cif
_cod_data_source_block           Zn4-1-48ClO4
_cod_original_cell_volume        21295.0(16)
_cod_database_code               7042832
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.778
_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
2. Others
 Fixed Sof: O12(0.5) O13(0.5) O14(0.5) O15(0.5) O16(0.5) O17(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C18(H18A,H18B), C25(H25A,H25B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), N5(H5), C5(H5A), N6(H6), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
  C15(H15), C20(H20), C21(H21), C22(H22), C24(H24), C28(H28), C29(H29),
 C30(H30), C33(H33), C36(H36), C37(H37), C39(H39), C40(H40)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              26267
_shelx_fab_checksum              22695
_olex2_submission_special_instructions 'No special instructions were received'