(<i>E</i>)-6,6'-(Diazene-1,2-diyl)bis(1,10-phenanthrolin-5-ol) trichloromethane disolvate: a superconjugated ligand
Ahmed, Muhib; Devereux, Michael; McKee, Vickie; McCann, Malachy; Rooney, A. Denise; Acta Crystallographica Section E 75 (2019) 1224–1227; doi:10.1107/S205698901900954X

data_2243030
_publ_section_title
;
 (<i>E</i>)-6,6'-(Diazene-1,2-diyl)bis(1,10-phenanthrolin-5-ol)
 trichloromethane disolvate: a superconjugated ligand
;
_journal_coeditor_code           JJ2213
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1224
_journal_page_last               1227
_journal_paper_doi               10.1107/S205698901900954X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C24 H14 N6 O2, 2C H Cl3'
_chemical_formula_moiety         'C24 H14 N6 O2, 2(C H Cl3)'
_chemical_formula_sum            'C26 H16 Cl6 N6 O2'
_chemical_formula_weight         657.15
_chemical_name_systematic
;
(<i>E</i>)-6,6'-(Diazene-1,2-diyl)bis(1,10-phenanthrolin-5-ol)
trichloromethane disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 96.863(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.9406(7)
_cell_length_b                   18.856(2)
_cell_length_c                   12.2375(16)
_cell_measurement_reflns_used    5155
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.73
_cell_volume                     1361.0(3)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker--Nonius X8 APEXII CCD'
_diffrn_measurement_method       'thin-slice \w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18529
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.167
_diffrn_reflns_theta_min         2.735
_diffrn_source                   'fine-focus sealed-tube'
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2012)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       lath
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.593
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    heteroxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0444P)^2^+1.8407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                2068
_reflns_number_total             2732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jj2213sup1.cif
_cod_data_source_block           I
_cod_database_code               2243030
_cod_database_fobs_code          2243030
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.974
_shelx_hkl_checksum              64982
_shelx_res_checksum              77885