Structural studies of Schiff-base [2 + 2] macrocycles derived from 2,2'-oxydianiline and the ROP capability of their organoaluminium complexes.
Yang, Wenxue; Zhao, Ke-Qing; Prior, Timothy J.; Hughes, David L.; Arbaoui, Abdessamad; Elsegood, Mark R. J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11990–12005; doi:10.1039/c6dt01997h

data_7039837
_publ_section_title
;
 Structural studies of Schiff-base [2 + 2] macrocycles derived from
 2,2'-oxydianiline and the ROP capability of their organoaluminium
 complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11990
_journal_page_last               12005
_journal_paper_doi               10.1039/c6dt01997h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C48 H44 N4 O4, 2(C7 H8)'
_chemical_formula_structural     'L2H2, 2(toluene) '
_chemical_formula_sum            'C62 H60 N4 O4'
_chemical_formula_weight         925.14
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
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_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-15 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.428(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8127(5)
_cell_length_b                   16.8060(6)
_cell_length_c                   22.5196(9)
_cell_measurement_reflns_used    5482
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      26.3010
_cell_measurement_theta_min      3.7090
_cell_volume                     5039.2(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies, Version 1.171.37.35 
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CrysAlisPro, Agilent Technologies, Version 1.171.37.35 
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CrysAlisPro, Agilent Technologies, Version 1.171.37.35 
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
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_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -25
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_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70863
_exptl_absorpt_correction_type   multi-scan
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         8856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0677P)^2^+0.8423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6118
_reflns_number_total             8856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01997h2.cif
_cod_data_source_block           yxqb
_cod_depositor_comments
'Adding full bibliography for 7039831--7039842.cif.'
_cod_database_code               7039837
_shelx_shelxl_version_number     2014/7
_shelxl_version_number           2013-4
_shelx_res_checksum              11574