Coordination-driven self-assembly of a series of dinuclear M<sub>2</sub>L<sub>2</sub> mesocates with a bis-bidentate pyridylimine ligand.
Chainok, Kittipong; Jittirattanakun, Siripak; Theppitak, Chatphorn; Jiajaroen, Suwadee; Puangsing, Praifon; Saphu, Watcharin; Kielar, Filip; Dungkaew, Winya; Rungtaweevoranit, Bunyarat; Sukwattanasinitt, Mongkol; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7736–7743; doi:10.1039/d1dt00146a

data_7707243
_publ_section_title
;
 Coordination-driven self-assembly of a series of dinuclear
 M<sub>2</sub>L<sub>2</sub> mesocates with a bis-bidentate pyridylimine
 ligand.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7736
_journal_page_last               7743
_journal_paper_doi               10.1039/d1dt00146a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C64 H44 N12 O4 S4 Zn2), 9(C H4 O)'
_chemical_formula_sum            'C137 H124 N24 O17 S8 Zn4'
_chemical_formula_weight         2896.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-01 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.8210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.1589(5)
_cell_length_b                   13.9590(4)
_cell_length_c                   24.6924(9)
_cell_measurement_reflns_used    9487
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.207
_cell_measurement_theta_min      4.197
_cell_volume                     6861.0(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31972
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.200
_diffrn_reflns_theta_min         4.442
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1389 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.7373.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00195(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6658
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1224P)^2^+30.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6579
_reflns_number_total             6658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00146a2.cif
_cod_data_source_block           1zn
_cod_depositor_comments
'Adding full bibliography for 7707240--7707244.cif.'
_cod_database_code               7707243
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.518
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 O5, C35
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O4, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O5(0.25) HB(0.25) C35(0.25) HI(0.25) HJ(0.25) HK(0.25)
5.a Riding coordinates:
 O3(H), O5(HB), C33(HC,HD,HE)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
 C34(HF,HG,HH), C35(HI,HJ,HK)
5.d Idealised tetrahedral OH refined as rotating group:
 O4(HA)
;
_shelx_res_checksum              81900
_olex2_submission_special_instructions 'No special instructions were received'