Metalloligands based on Robson-type amino-thiophenolato macrocycles for assembly of heterotrimetallic complexes.
Schmorl, Sara; Naumov, Sergej; Abel, Bernd; Börner, Martin; Pöppl, Andreas; Kersting, Berthold; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5784–5788; doi:10.1039/d1dt00723h

data_7707127
_publ_section_title
;
 Metalloligands based on Robson-type amino-thiophenolato macrocycles for
 assembly of heterotrimetallic complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5784
_journal_page_last               5788
_journal_paper_doi               10.1039/d1dt00723h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C38 H64 Cu F I2 N6 Ni2 S2, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H70 Cu F I2 N8 Ni2 S2'
_chemical_formula_weight         1204.94
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                92.79(3)
_cell_angle_beta                 108.39(3)
_cell_angle_gamma                110.92(3)
_cell_formula_units_Z            2
_cell_length_a                   13.171(3)
_cell_length_b                   13.363(3)
_cell_length_c                   15.858(3)
_cell_measurement_reflns_used    35502
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.55
_cell_volume                     2432.6(12)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE X-AREA'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device       '1-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24771
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         2.527
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.596
_exptl_absorpt_correction_T_max  0.7753
_exptl_absorpt_correction_T_min  0.5568
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.169
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0551P)^2^+1.9144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9181
_reflns_number_total             10418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00723h2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707127.cif.
;
_cod_database_code               7707127
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.576
_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 Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), N6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C18(H18), C20(H20)
2.d Idealised Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              27947
_shelx_hkl_checksum              28787
_olex2_submission_special_instructions 'No special instructions were received'