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_7707244
_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 Fe2 N12 O4 S4), 9(C H4 O)'
_chemical_formula_sum            'C137 H124 Fe4 N24 O17 S8'
_chemical_formula_weight         2858.47
_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             2020-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-01 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.6680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.0043(6)
_cell_length_b                   13.9622(4)
_cell_length_c                   24.3765(7)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.243
_cell_measurement_theta_min      3.876
_cell_volume                     6731.7(3)
_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_detector                 'PHOTON 200 CMOS DETECTOR'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'PHOTON 200 CMOS'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '\k-Geometry Diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30127
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.256
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'X-ray tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_target            Cu
_diffrn_source_type              'Micro focus tube'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.154
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1097 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.5816.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       rod
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00117(16)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6493
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0892P)^2^+34.1324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6124
_reflns_number_total             6493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00146a2.cif
_cod_data_source_block           1fe
_cod_depositor_comments
'Adding full bibliography for 7707240--7707244.cif.'
_cod_database_code               7707244
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.307
_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, All O(H,H) groups
2. Restrained distances
 O5-C35
 1.4 with sigma of 0.001
 O4-C34 \\sim O4-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(C34A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. 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
 O4, C34A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H4B)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(H4A)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Fixed Sof: O5(0.25) H5A(0.25) C35(0.25) H35A(0.25) H35B(0.25) H35C(0.25)
6.a Riding coordinates:
 O3(H3A), O5(H5A), C35(H35A,H35B,H35C)
6.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)
6.c Tetrahedral OH refined with riding coordinates:
 O4(H4A), O4(H4B)
6.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              14535
_olex2_submission_special_instructions 'No special instructions were received'