Carbazole-based N4-donor Schiff base macrocycles: obtained metal free and as Cu(ii) and Ni(ii) complexes.
Malthus, Stuart J.; Wilson, Rajni K.; Vikas Aggarwal, A.; Cameron, Scott A.; Larsen, David S.; Brooker, Sally; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3141–3149; doi:10.1039/c6dt04598g

data_7041790
_publ_section_title
;
 Carbazole-based N4-donor Schiff base macrocycles: obtained metal free and
 as Cu(ii) and Ni(ii) complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3141
_journal_page_last               3149
_journal_paper_doi               10.1039/c6dt04598g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C22 H26 N4 Ni O3'
_chemical_formula_weight         453.18
_chemical_name_systematic        'Ni(II) carbazole Schiff-base macrocycle'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6646(3)
_cell_length_b                   12.9442(4)
_cell_length_c                   23.1878(7)
_cell_measurement_reflns_used    8929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1310
_cell_measurement_theta_min      5.0910
_cell_volume                     2000.36(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction Supernova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13219
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.285
_diffrn_reflns_theta_min         5.121
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_preparation       ', redox, NMR'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.69218
_refine_diff_density_max         1.598
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 1419 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.48(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+11.5403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2532
_refine_ls_wR_factor_ref         0.2554
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                3910
_reflns_number_total             4086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04598g2.cif
_cod_data_source_block           SXM_385
_cod_depositor_comments
'Adding full bibliography for 7041789--7041790.cif.'
_cod_database_code               7041790
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.921
_shelx_res_checksum              64950