Selective synthesis of a heterotetranuclear complex from a macrocyclic ligand with multiple identical chelating units.
Seki, Kota; Nakamura, Takashi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6034–6037; doi:10.1039/d5dt00623f

data_7718445
_publ_section_title
;
 Selective synthesis of a heterotetranuclear complex from a macrocyclic
 ligand with multiple identical chelating units.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6034
_journal_page_last               6037
_journal_paper_doi               10.1039/d5dt00623f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'(C78 H74 F12 Mo2 N4 O14), 5.5(C H Cl3), 2(C4 H8 O)'
_chemical_formula_sum            'C91.5 H95.5 Cl16.5 F12 Mo2 N4 O16'
_chemical_formula_weight         2512.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-02-15 deposited with the CCDC.	2025-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.4270(10)
_cell_angle_beta                 90.6740(10)
_cell_angle_gamma                107.2210(10)
_cell_formula_units_Z            2
_cell_length_a                   14.7987(4)
_cell_length_b                   17.5747(5)
_cell_length_c                   22.7001(6)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.640
_cell_measurement_theta_min      2.168
_cell_volume                     5532.7(3)
_computing_cell_refinement       'APEX3 (Bruker Nano, 2019)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'APEX3 (Bruker Nano, 2019)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            375917
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;    
 SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       column
_exptl_crystal_F_000             2546
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         4.406
_refine_diff_density_min         -1.615
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1437
_refine_ls_number_reflns         25358
_refine_ls_number_restraints     307
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1341P)^2^+43.7226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2438
_refine_ls_wR_factor_ref         0.2775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19361
_reflns_number_total             25358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00623f2.cif
_cod_data_source_block           s100a_a
_cod_depositor_comments
'Adding full bibliography for 7718442--7718445.cif.'
_cod_original_formula_sum        'C91.50 H95.50 Cl16.50 F12 Mo2 N4 O16'
_cod_database_code               7718445
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              30036
_shelx_hkl_checksum              54267