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_7707356
_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         'C52 H52 Br Fe N4 O2, Br, 5.5[CH3CN]'
_chemical_formula_sum            'C52 H52 Br2 Fe N4 O2'
_chemical_formula_weight         980.64
_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             2021-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-04-28 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.484(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2077(6)
_cell_length_b                   27.6241(9)
_cell_length_c                   15.1579(8)
_cell_measurement_reflns_used    16199
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      2.148
_cell_measurement_theta_min      27.526
_cell_volume                     5496.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47911
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.55484
_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_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.901
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.110
_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     556
_refine_ls_number_reflns         12466
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0724P)^2^+20.1735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9446
_reflns_number_total             12466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           ferop3
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_database_code               7707356
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.657
_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 Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C44(H44A,H44B), C45(H45A,H45B)
2.b 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), N3(H3A)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 496 electrons were 
found in a volume of 1544\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
5.5[CH3CN] per Asymmetric Unit 
which account for 484 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97911
_shelx_fab_checksum              12188
_olex2_submission_special_instructions 'No special instructions were received'