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_7042831
_publ_section_title
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 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         'C42 H36 Cu2 N14 O18, 5(C2 H3 N)'
_chemical_formula_sum            'C52 H51 Cu2 N19 O18'
_chemical_formula_weight         1357.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.688(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4413(8)
_cell_length_b                   29.901(2)
_cell_length_c                   15.8843(10)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.16
_cell_volume                     5906.5(7)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_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 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            75015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.999
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.452
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.8757.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         11613
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0530P)^2^+17.9250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8111
_reflns_number_total             11613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01533j2.cif
_cod_data_source_block           Cu2NO341
_cod_original_cell_volume        5906.6(7)
_cod_database_code               7042831
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.895
_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. Restrained distances
 C52-C51 \\sim C54-C53
 with sigma of 0.01
 N20-C54 \\sim N19-C52
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N19) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(N20) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
Uanis(C51) = Uanis(C53)
4. Others
 Fixed Sof: N20(0.4) C53(0.4) H53A(0.4) H53B(0.4) H53C(0.4) C54(0.4) N19(0.6)
 C51(0.6) H51A(0.6) H51B(0.6) H51C(0.6) C52(0.6)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C18(H18A,H18B), C25(H25A,H25B), C34(H34A,H34B)
5.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), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29),
 C30(H30), C33(H33), C36(H36), C37(H37), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C53(H53A,H53B,
 H53C), C51(H51A,H51B,H51C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C47(H47A,
 H47B,H47C)
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_shelx_res_checksum              92405
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'