Iron homo- and heterobimetallic complexes supported by a symmetrical dinucleating ligand.
Ríos, Pablo; See, Matthew S.; Gonzalez, Oscar; Handford, Rex C.; Nicolay, Amélie; Rao, Guodong; Britt, R. David; Bediako, D. Kwabena; Tilley, T. Don; Chemical communications (Cambridge, England) 60 (2024) 8912–8915; doi:10.1039/d4cc02155j

data_7133379
_publ_section_title
;
 Iron homo- and heterobimetallic complexes supported by a symmetrical
 dinucleating ligand.
;
_journal_issue                   67
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8912
_journal_page_last               8915
_journal_paper_doi               10.1039/d4cc02155j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'0.047(C90 H84 Cl2 Fe2 N24), 0.093(C F3 O3 S), 0.093(C2 H3 N), 0.047[C4H10OC2H3N]'
_chemical_formula_sum            'C96 H90 Cl2 F6 Fe2 N26 O6 S2'
_chemical_formula_weight         2064.65
_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     dual
_audit_creation_date             2023-10-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-17 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                78.520(3)
_cell_angle_beta                 74.856(3)
_cell_angle_gamma                72.035(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0576(10)
_cell_length_b                   19.1460(14)
_cell_length_c                   22.1777(16)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.863
_cell_measurement_theta_min      2.837
_cell_volume                     5435.1(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            77076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.933
_diffrn_reflns_theta_min         1.418
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       needle
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         21664
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1152P)^2^+3.3093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17288
_reflns_number_total             21664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02155j2.cif
_cod_data_source_block           pr382_0m
_cod_depositor_comments
'Adding full bibliography for 7133376--7133380.cif.'
_cod_database_code               7133379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.987
_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
2. Rigid body (RIGU) restrains
 C60, C93, C89, C61, C87, C62, C91, C63, C86, C64, C88, C65, C90, C79, C92,
 C82, C94, C85
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C96, C112, C108, C97, C106, C98, C110, C99, C105, C100, C107, C101, C109,
 C102, C111, C103, C113, C104
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=Sof(C97)=Sof(C98)=Sof(H98)=Sof(C99)=
 Sof(C100)=Sof(H100)=Sof(C101)=Sof(C102)=Sof(C103)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C104)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=
 Sof(C87)=Sof(C88)=Sof(C89)=Sof(C90)=Sof(H90)=Sof(C91)=Sof(C92)=Sof(H92)=
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=FVAR(1)
 Sof(C105)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C106)=Sof(C107)=Sof(H107)=
 Sof(C108)=Sof(C109)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C110)=Sof(H110)=
 Sof(C111)=Sof(C112)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C113)=1-FVAR(2)
 Sof(C60)=Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C18(H18), C21(H21), C23(H23), C25(H25), C26(H26),
 C27(H27), C28(H28), C30(H30), C32(H32), C34(H34), C35(H35), C37(H37), C39(H39),
  C40(H40), C52(H52), C56(H56), C57(H57), C59(H59), C62(H62), C64(H64),
 C66(H66), C68(H68), C70(H70), C72(H72), C77(H77), C90(H90), C92(H92), C98(H98),
  C100(H100), C107(H107), C110(H110)
4.b Fitted hexagon refined as free rotating group:
 C87(C88,C89,C90,C91,C92), C97(C98,C99,C100,C101,C102)
4.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C1A(H1AA,H1AB,H1AC), C58(H58A,H58B,H58C), C69(H69A,
 H69B,H69C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C82(H82A,H82B,
 H82C), C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C103(H10A,H10B,H10C),
 C104(H10D,H10E,H10F), C105(H10G,H10H,H10I), C109(H10J,H10K,H10L), C112(H11A,
 H11B,H11C)
;
_shelx_res_checksum              53458
_shelx_hkl_checksum              98848
_shelx_fab_checksum              91735
_olex2_submission_special_instructions 'No special instructions were received'