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_7707347
_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 H54 N4 O2, Br4 Co [+ 2MeCN]
;
_chemical_formula_sum            'C52 H54 Br4 Co N4 O2'
_chemical_formula_weight         1145.56
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                96.850(3)
_cell_angle_beta                 91.115(3)
_cell_angle_gamma                99.672(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2629(5)
_cell_length_b                   13.2489(6)
_cell_length_c                   17.0384(7)
_cell_measurement_reflns_used    12439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.684
_cell_measurement_theta_min      2.02
_cell_volume                     2707.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and 
an AFC12 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10619
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        21.726
_diffrn_reflns_theta_max         21.726
_diffrn_reflns_theta_min         1.571
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.65216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;

Composition is 

 C52 H54 N4 O2, Br4 Co [+ 2MeCN]

with the squeeze solvent included in this the composition is:

 C56 H60 N6 O2, Br4 Co 
;
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10619
_refine_ls_number_restraints     839
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.1136
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+88.8486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2782
_refine_ls_wR_factor_ref         0.2974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9065
_reflns_number_total             10619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           FeROP6
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_database_code               7707347
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.733
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              70524
_shelx_fab_checksum              32956