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_7707354
_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(C46 H40 Br Fe N4 O2), 2(C2 H3 N), Br6 Fe2 O'
_chemical_formula_sum            'C96 H86 Br8 Fe4 N10 O5'
_chemical_formula_weight         2322.42
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2021-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.896(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6606(4)
_cell_length_b                   16.0326(4)
_cell_length_c                   37.4062(11)
_cell_measurement_reflns_used    8333
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      67.1860
_cell_measurement_theta_min      2.8890
_cell_volume                     9252.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.14
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  23.00   0.50   10.00    --    5.00   8.00 -14.00   70
  2  \w    -28.00  89.00   0.50   10.00    --    0.00  57.00  90.00  234
  3  \w    -87.00 -38.00   0.50   10.00    --    0.00  57.00  90.00   98
  4  \w   -162.00  -4.00   0.50   40.00    --  -90.00   8.00 -14.00  316
  5  \w   -172.00-146.00   0.50   40.00    --  -90.00  43.00 -30.00   52
  6  \w   -137.00-110.00   0.50   40.00    --  -90.00  43.00 -30.00   54
  7  \w   -141.00 -82.00   0.50   40.00    --  -90.00  57.00 -30.00  118
  8  \w    -38.00 -12.00   0.50   40.00    --  -90.00  57.00 -30.00   52
  9  \w   -179.00 -83.00   0.50   40.00    --  -90.00  57.00-180.00  192
 10  \w    -50.00 -12.00   0.50   40.00    --  -90.00  57.00-180.00   76
 11  \w   -178.00-145.00   0.50   40.00    --  -90.00  57.00 -30.00   66
 12  \w   -179.00 -86.00   0.50   40.00    --  -90.00  57.00-150.00  186
 13  \w   -141.00  -1.00   0.50   40.00    --  -90.00  60.00  60.00  280
 14  \w   -133.00 -83.00   0.50   40.00    --  -90.00  60.00 150.00  100
 15  \w    -65.00 -39.00   0.50   40.00    --  -90.00  60.00 -60.00   52
 16  \w   -179.00-145.00   0.50   40.00    --  -90.00  60.00 150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0642516000
_diffrn_orient_matrix_UB_12      0.0032284000
_diffrn_orient_matrix_UB_13      0.0361068000
_diffrn_orient_matrix_UB_21      0.0752689000
_diffrn_orient_matrix_UB_22      0.0139140000
_diffrn_orient_matrix_UB_23      -0.0209892000
_diffrn_orient_matrix_UB_31      -0.0130809000
_diffrn_orient_matrix_UB_32      0.0950512000
_diffrn_orient_matrix_UB_33      0.0018606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            68070
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.909
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       plate
_exptl_crystal_F_000             4624
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         16805
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0877P)^2^+1.8599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9942
_reflns_number_total             16805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00711d2.cif
_cod_data_source_block           FeROP1
_cod_depositor_comments
'Adding full bibliography for 7707347--7707359.cif.'
_cod_database_code               7707354
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C96 H86 Br8 Fe4 N10 O5'
_chemical_oxdiff_usercomment     FeMeEhtyl
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.519
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Restrained distances
 Fe3-Br4 \\sim Fe3-Br5 \\sim Fe3-Br3 \\sim Fe3-Br3A \\sim Fe3-Br4A \\sim
Fe3-Br5A
 with sigma of 0.02
 Br3-Br4 \\sim Br4-Br5 \\sim Br5-Br3
 with sigma of 0.02
3. Others
 Sof(Br5A)=Sof(Fe3A)=Sof(Br4A)=Sof(Br3A)=1-FVAR(1)
 Sof(Br3)=Sof(Br4)=Sof(Br5)=Sof(Fe3)=FVAR(1)
 Fixed Uiso: Br5A(0.065) Fe3A(0.028) Br4A(0.065) Br3A(0.065)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C38(H38A,H38B), C39(H39A,H39B), C65(H65A,
 H65B), C66(H66A,H66B), C88(H88A,H88B), C89(H89A,H89B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C26(H26), C28(H28),
  C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), N6(H6), N8(H8A), C53(H53), C55(H55), C58(H58),
 C60(H60), C61(H61), C62(H62), C63(H63), C68(H68), C69(H69), C70(H70), C71(H71),
  C73(H73), C76(H76), C78(H78), C81(H81), C83(H83), C84(H84), C85(H85),
 C86(H86), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C30(H30A,H30B,H30C), C57(H57A,H57B,H57C), C80(H80A,H80B,
 H80C), C102(H10A,H10B,H10C), C104(H10D,H10E,H10F)
;
_shelx_res_checksum              93894
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.759