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_7123872
_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         '2(C30 H34 N4 O2 Si2)'
_chemical_formula_sum            'C60 H68 N8 O4 Si4'
_chemical_formula_weight         1077.58
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-24 deposited with the CCDC.    2019-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                102.4020(10)
_cell_angle_beta                 98.165(2)
_cell_angle_gamma                106.5800(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7552(4)
_cell_length_b                   13.6950(4)
_cell_length_c                   20.8774(6)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.74
_cell_measurement_theta_min      3.50
_cell_volume                     3070.98(17)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35417
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.913
_diffrn_reflns_theta_min         2.220
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.7571. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1150P)^2^+0.5650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10172
_reflns_number_total             11490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03316e2.cif
_cod_data_source_block           4
_cod_database_code               7123872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.510
_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.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C19(H19A,H19B), C49(H49A,H49B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N4(H4), N2(H2), N8(H8), C4(H4A), C34(H34), C10(H10), C24(H24),
 C22(H22), C36(H36), C1(H1), C6(H6A), C42(H42), C32(H32), C11(H11), C31(H31),
 C40(H40), C41(H41), C12(H12), C23(H23), C2(H2A), C52(H52), C53(H53), C54(H54)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C28(H28A,H28B,
 H28C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C30(H30A,
 H30B,H30C), C29(H29A,H29B,H29C), C60(H60A,H60B,H60C), C59(H59A,H59B,H59C),
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              17510
_olex2_submission_special_instructions 'No special instructions were received'