Unexpected linkage isomerism in chiral tetranuclear bis-tridentate (1,2,3-triazol-4-yl)-picolinamide (tzpa) grids
Hegarty, Isabel; Dalton, Hannah L.; Henwood, Adam; Hawes, Chris Samuel; Gunnlaugsson, Thorfinnur; Chemical Communications  (2019) –; doi:10.1039/C9CC03316E

data_7123874
_publ_section_title
;
 Unexpected linkage isomerism in chiral tetranuclear bis-tridentate
 (1,2,3-triazol-4-yl)-picolinamide (tzpa) grids
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03316E
_journal_year                    2019
_chemical_formula_moiety         'C40 H36 Cu2 N14 O14, C2 H3 N'
_chemical_formula_sum            'C42 H39 Cu2 N15 O14'
_chemical_formula_weight         1104.96
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-24 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.288(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6908(16)
_cell_length_b                   12.2647(6)
_cell_length_c                   15.4847(8)
_cell_measurement_reflns_used    3255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.38
_cell_measurement_theta_min      3.61
_cell_volume                     4651.3(5)
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2490
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49115
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        56.908
_diffrn_reflns_theta_max         56.908
_diffrn_reflns_theta_min         1.804
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.857
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1221 before and 0.0879 after correction. The Ratio of minimum to maximum transmission is 0.6999. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         6255
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1847
_refine_ls_R_factor_gt           0.1298
_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^)+(0.1271P)^2^+59.4364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2913
_refine_ls_wR_factor_ref         0.3186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3859
_reflns_number_total             6255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03316e2.cif
_cod_data_source_block           Cu2H21NO34MeCN
_cod_database_code               7123874
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.781
_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. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, N9, N10, C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Ternary CH refined with riding coordinates:
 C7(H7), C33(H33)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C24(H24A,H24B)
4.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C34(H34A,H34B,H34C)
4.d Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C2(H2), C1(H1), C5(H5A), C4(H4), C3(H3), C9(H9), C12(H12),
 C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28),
  C29(H29), C32(H32), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
4.e Fitted hexagon refined as free rotating group:
 C2(C1,C6,C5,C4,C3), C35(C36,C37,C38,C39,C40)
4.f Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
;
_shelx_res_checksum              79047
_olex2_submission_special_instructions 'No special instructions were received'