Coordination chemistry of [2 + 2] Schiff-base macrocycles derived from the dianilines [(2-NH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>2</sub>X] (X = CH<sub>2</sub>CH<sub>2</sub>, O): structural studies and ROP capability towards cyclic esters.
Wang, Kuiyuan; Prior, Timothy J.; Hughes, David L.; Arbaoui, Abdessamad; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8057–8069; doi:10.1039/d1dt00711d

data_7707358
_publ_section_title
;
 Coordination chemistry of [2 + 2] Schiff-base macrocycles derived from
 the dianilines
 [(2-NH<sub>2</sub>C<sub>6</sub>H<sub>4</sub>)<sub>2</sub>X] (X =
 CH<sub>2</sub>CH<sub>2</sub>, O): structural studies and ROP capability
 towards cyclic esters.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8057
_journal_page_last               8069
_journal_paper_doi               10.1039/d1dt00711d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '2(C52 H52 Br Fe N4 O2), C2 H3 N, Br6 Fe2 O'
_chemical_formula_sum            'C106 H107 Br8 Fe4 N9 O5'
_chemical_formula_weight         2449.68
_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             2021-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                67.263(5)
_cell_angle_beta                 88.642(4)
_cell_angle_gamma                81.638(4)
_cell_formula_units_Z            1
_cell_length_a                   13.6454(5)
_cell_length_b                   13.9070(7)
_cell_length_c                   15.6432(8)
_cell_measurement_reflns_used    20939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.114
_cell_measurement_theta_min      27.504
_cell_volume                     2707.0(2)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12337
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.531
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5920
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         12337
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0697P)^2^+8.1221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8627
_reflns_number_total             12337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           FeROP2
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_database_code               7707358
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.417
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.840(5)
 0.160(5)
2. 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
3. Restrained distances
 Fe2-Br2A \\sim Fe2-Br2B \\sim Fe2-Br4A \\sim Fe2-Br4B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Br2A) = Uanis(Br2B)
Uanis(Br4A) = Uanis(Br4B)
5. Others
 Sof(Br2B)=Sof(Br4B)=1-FVAR(1)
 Sof(Br2A)=Sof(Br4A)=FVAR(1)
 Fixed Sof: N5(0.5) C61(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C44(H44A,H44B), C45(H45A,H45B)
6.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C29(H29), C31(H31), C37(H37), C39(H39),
  C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50),
 C52(H52), N2(H2), N4(H4)
6.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              88479
_olex2_submission_special_instructions 'No special instructions were received'