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_7133377
_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         '2(C30 H28 N8), 0.5(C4 H10 O), O'
_chemical_formula_sum            'C62 H61 N16 O1.5'
_chemical_formula_weight         1054.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 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                 126.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0364(12)
_cell_length_b                   14.7281(7)
_cell_length_c                   19.7560(16)
_cell_measurement_reflns_used    9466
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.56
_cell_volume                     5639.2(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37779
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.105
_diffrn_reflns_theta_min         1.738
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1265 before and 0.0851 after correction.
The Ratio of minimum to maximum transmission is 0.8911.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             2228
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 4234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(6)
_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     754
_refine_ls_number_reflns         10320
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0809P)^2^+6.5676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                9650
_reflns_number_total             10320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02155j2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7133376--7133380.cif.'
_cod_original_formula_sum        'C62 H61 N16 O1.50'
_cod_database_code               7133377
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.980
_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
 O1-C61
 1.41 with sigma of 0.02
 O1-C62
 1.42 with sigma of 0.02
 C60-C61
 1.48 with sigma of 0.02
 C62-C63
 1.5 with sigma of 0.02
 O1-C60 = O1-C63
 2.37 with sigma of 0.04
 C60-C61 \\sim C62-C63
 with sigma of 0.02
 O1-C61 \\sim O1-C62
 with sigma of 0.02
 C60-O1 \\sim O1-C63
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C63 \\sim O1 \\sim C61 \\sim C62 \\sim C60: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O1, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5)
 H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C17(H17), C20(H20), C22(H22), C23(H23), C26(H26), C28(H28),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C45(H45),
  C46(H46), C48(H48), C49(H49), C58(H58)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C1A(H1AA,H1AB,H1AC), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              16695
_shelx_hkl_checksum              95261
_olex2_submission_special_instructions 'No special instructions were received'