Accessing bimetallic complexes through a variable bridging ligand strategy.
Liyanage, Hansani T Lekam Wasam; Smith, Mark D.; Wheeler, Kraig A.; Semeniuc, Radu F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1063–1078; doi:10.1039/d4dt02903h

data_7717574
_publ_section_title
;
 Accessing bimetallic complexes through a variable bridging ligand
 strategy.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1063
_journal_page_last               1078
_journal_paper_doi               10.1039/d4dt02903h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '0.28(H2 O), 0.229(O1), 2(C19 H16 Cu N6 O3)'
_chemical_formula_sum            'C38 H32.56 Cu2 N12 O6.51'
_chemical_formula_weight         888.56
_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   mixed
_audit_creation_date             2024-11-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-13 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                114.194(3)
_cell_angle_beta                 93.294(3)
_cell_angle_gamma                103.183(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6542(6)
_cell_length_b                   13.8554(8)
_cell_length_c                   16.0283(9)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.302
_cell_measurement_theta_min      3.597
_cell_volume                     1876.4(2)
_computing_cell_refinement       'SAINT+ V8.40B (Bruker AXS Inc., 2020)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ve8.40B (Bruker-AXS, 2020)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2019/1)'
_computing_structure_solution    'XT (Sheldrick, 2018/2)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX II CCD'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       '\three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirror'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'multilayer mirror'
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42460
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         3.067
_diffrn_source                   'fine focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             909
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         6721
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0270P)^2^+3.9450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6029
_reflns_number_total             6721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02903h2.cif
_cod_data_source_block           16rfs09
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717572--7717578.cif.
;
_cod_database_code               7717574
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.602
_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,H) groups
2. Restrained distances
 Cu1B-O2C \\sim Cu1B-O2B
 with sigma of 0.02
 O2C-C18C \\sim O2B-C18B
 with sigma of 0.02
 O3C-C18C \\sim O3B-C18B
 with sigma of 0.02
 C18C-C19C \\sim C18B-C19B
 with sigma of 0.02
 Cu1B-C18C \\sim Cu1B-C18B
 with sigma of 0.04
 O2C-O3C \\sim O2B-O3B
 with sigma of 0.04
 O2C-C19C \\sim O2B-C19B
 with sigma of 0.04
 O3C-C19C \\sim O3B-C19B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O4A) \\sim Ueq, Uanis(O4B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O2C) = Uanis(O2B)
Uanis(O3C) = Uanis(O3B)
Uanis(C18C) = Uanis(C18B)
4. Rigid body (RIGU) restrains
 O2C, O3C, C18C, C19C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, O3B, C18B, C19B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, O3B, C18B, C19B, O2C, O3C, C18C, C19C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(O2C)=Sof(O3C)=Sof(C18C)=Sof(C19C)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(O2B)=Sof(O3B)=Sof(C18B)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(O1)=Sof(H1C)=Sof(H1D)=FVAR(2)
6.a Free rotating group:
 O1(H1C,H1D)
6.b Ternary CH refined with riding coordinates:
 C11A(H11A), C11B(H11B)
6.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C1B(H1B), C2B(H2B),
  C3B(H3B), C5B(H5B), C6B(H6B), C7B(H7B), C12B(H12B), C13B(H13B), C14B(H14B),
 C15B(H15B), C16B(H16B), C17B(H17B)
6.d Idealised Me refined as rotating group:
 C19A(H19G,H19H,H19I), C19B(H19A,H19B,H19C), C19C(H19D,H19E,H19F)
;
_shelx_res_checksum              70813
_shelx_hkl_checksum              10311
_olex2_submission_special_instructions 'No special instructions were received'