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_7133376
_publ_section_title
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 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
'C68 H72 Cl Fe2 N16 O2, 3(C2 F6 N O4 S2), 2(C4 H8 O)'
_chemical_formula_sum            'C82 H88 Cl F18 Fe2 N19 O16 S6'
_chemical_formula_weight         2277.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-09 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5489(5)
_cell_length_b                   15.0572(5)
_cell_length_c                   36.9438(11)
_cell_measurement_reflns_used    9443
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      2.20
_cell_volume                     9725.5(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            158657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.143
_diffrn_reflns_theta_min         1.885
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0859 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.9281.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1627
_refine_ls_number_reflns         24249
_refine_ls_number_restraints     778
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+10.3355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18846
_reflns_number_total             24249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02155j2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7133376--7133380.cif.'
_cod_database_code               7133376
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C83-F19 = C83-F20 = C83-F22 = C84-F1A
 1.33 with sigma of 0.02
 C83-S7 = C84-S8
 1.84 with sigma of 0.02
 C84-F21
 1.34 with sigma of 0.02
 C84-F23
 1.3 with sigma of 0.02
 N19-S7
 1.58 with sigma of 0.02
 N19-S8
 1.56 with sigma of 0.02
 O17-S7
 1.42 with sigma of 0.02
 O18-S8 = O19-S8 = O1A-S7
 1.43 with sigma of 0.02
 C85-F24 = C85-F26 = C85-F28 = C86-F25
 1.33 with sigma of 0.02
 C85-S9 = C86-S10
 1.84 with sigma of 0.02
 C86-F27
 1.34 with sigma of 0.02
 C86-F29
 1.3 with sigma of 0.02
 N1A-S9
 1.58 with sigma of 0.02
 N1A-S10
 1.56 with sigma of 0.02
 O20-S9
 1.42 with sigma of 0.02
 O21-S10 = O22-S10 = O23-S9
 1.43 with sigma of 0.02
 C83-N19
 2.61 with sigma of 0.04
 C83-O17 = C84-O18
 2.58 with sigma of 0.04
 C83-O1A = N19-O17
 2.57 with sigma of 0.04
 C84-N19
 2.7 with sigma of 0.04
 C84-O19
 2.59 with sigma of 0.04
 N19-O1A = O18-O19
 2.48 with sigma of 0.04
 N19-O18
 2.54 with sigma of 0.04
 N19-O19
 2.4 with sigma of 0.04
 O17-O1A
 2.44 with sigma of 0.04
 C85-N1A
 2.61 with sigma of 0.04
 C85-O20 = C86-O21
 2.58 with sigma of 0.04
 C85-O23 = N1A-O20
 2.57 with sigma of 0.04
 C86-N1A
 2.7 with sigma of 0.04
 C86-O22
 2.59 with sigma of 0.04
 N1A-O23 = O21-O22
 2.48 with sigma of 0.04
 N1A-O21
 2.54 with sigma of 0.04
 N1A-O22
 2.4 with sigma of 0.04
 O20-O23
 2.44 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N18 \\sim S4 \\sim O10 \\sim O11 \\sim C79 \\sim F6 \\sim F7 \\sim F9 \\sim S5
\\sim O13 \\sim O15 \\sim C81 \\sim F12 \\sim F13 \\sim F17 \\sim N17 \\sim S3
\\sim O9 \\sim O12 \\sim C80 \\sim S6 \\sim F8 \\sim F10 \\sim F11 \\sim O14
\\sim O16 \\sim C82 \\sim F14 \\sim F15 \\sim F16: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
C87 \\sim S1 \\sim O3 \\sim O4 \\sim N16 \\sim C49 \\sim S2 \\sim S11 \\sim F2
\\sim F3 \\sim F4 \\sim O6 \\sim O7 \\sim C64 \\sim O24 \\sim F1 \\sim F5 \\sim
F18 \\sim F30 \\sim F31: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C78 \\sim O5 \\sim C67 \\sim C68 \\sim C72: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
F22 \\sim C83 \\sim F19 \\sim F20 \\sim S7 \\sim N19 \\sim O17 \\sim O1A \\sim
S8 \\sim C84 \\sim O18 \\sim O19 \\sim F1A \\sim F21 \\sim F23: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
N1A \\sim C85 \\sim F24 \\sim F26 \\sim F28 \\sim S9 \\sim O20 \\sim O23 \\sim
S10 \\sim C86 \\sim O21 \\sim O22 \\sim F25 \\sim F27 \\sim F29: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C77 \\sim C74 \\sim C75 \\sim C76 \\sim O8: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 1.7A
4. Others
 Sof(S4)=Sof(F6)=Sof(O10)=Sof(F7)=Sof(O11)=Sof(F9)=Sof(C79)=Sof(S5)=Sof(F12)=
 Sof(O13)=Sof(F13)=Sof(O15)=Sof(C81)=Sof(F17)=Sof(N18)=1-FVAR(1)
 Sof(S3)=Sof(O9)=Sof(F8)=Sof(N17)=Sof(O12)=Sof(F10)=Sof(F11)=Sof(C80)=Sof(S6)=
 Sof(O14)=Sof(O16)=Sof(F14)=Sof(F15)=Sof(C82)=Sof(F16)=FVAR(1)
 Sof(S11)=Sof(O24)=Sof(F30)=Sof(C87)=Sof(F31)=1-FVAR(2)
 Sof(F5)=Sof(O6)=Sof(C64)=Sof(S2)=Sof(F18)=FVAR(2)
 Sof(C85)=Sof(C86)=Sof(F24)=Sof(F25)=Sof(F26)=Sof(F27)=Sof(F28)=Sof(F29)=
 Sof(N1A)=Sof(O20)=Sof(O21)=Sof(O22)=Sof(O23)=Sof(S9)=Sof(S10)=1-FVAR(3)
 Sof(C83)=Sof(C84)=Sof(F19)=Sof(F1A)=Sof(F20)=Sof(F21)=Sof(F22)=Sof(F23)=
 Sof(N19)=Sof(O17)=Sof(O18)=Sof(O19)=Sof(O1A)=Sof(S7)=Sof(S8)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C50(H50A,H50B), C54(H54A,H54B), C62(H62A,H62B), C66(H66A,
 H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C78(H78A,H78B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C11(H11), C12(H12), C15(H15), C16(H16), C19(H19), C21(H21),
 C24(H24), C26(H26), C36(H36), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44),
  C47(H47), C51(H51), C58(H58), C61(H61)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C1A(H1AA,H1AB,H1AC), C48(H48A,H48B,H48C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C),
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              53553
_shelx_hkl_checksum              8632
_olex2_submission_special_instructions 'No special instructions were received'