6,6'-Dimethoxy-2,2'-[(<i>E</i>,<i>E</i>')-(4-chloro-<i>m</i>-phenylene)bis(nitrilomethylidyne)]diphenol
Yamin, Bohari M.; Bakar, Siti Najihah A.; Kassim, Karimah; Bahron, Hadariah; Acta Crystallographica Section E 65 (2009) o2573–; doi:10.1107/S1600536809037386

data_2223354
_publ_section_title
6,6'-Dimethoxy-2,2'-[(<i>E</i>,<i>E</i>')-(4-chloro-<i>m</i>-phenylene)bis(nitrilomethylidyne)]diphenol
_journal_coeditor_code           DN2481
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2573
_journal_paper_doi               10.1107/S1600536809037386
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C22 H19 Cl N2 O4'
_chemical_formula_moiety         'C22 H19 Cl N2 O4'
_chemical_formula_sum            'C22 H19 Cl N2 O4'
_chemical_formula_weight         410.84
_chemical_melting_point_gt       468.0
_chemical_melting_point_lt       470.0
_chemical_name_systematic
;
6,6'-Dimethoxy-2,2'-[(<i>E</i>,<i>E</i>')-(4-chloro-<i>m</i>-
phenylene)bis(nitrilomethylidyne)]diphenol
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.659(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.900(2)
_cell_length_b                   6.8589(12)
_cell_length_c                   28.830(6)
_cell_measurement_reflns_used    2429
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      1.4
_cell_volume                     1951.2(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PARST (Nardelli, 1995) and PLATON
(Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 83.66
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD area-detector
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12204
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         1.4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4049
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.087
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.4146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                2758
_reflns_number_total             4049
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2481.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2223354
_cod_database_fobs_code          2223354