{<i>N,N</i>'-Bis[3-methoxymethyl-5-methylsalicylidene]-(<i>R,R</i>)-1,2-diphenylenediamino}nickel(II)
Jin-Cai Wu; Ning Tang; Kai-Bei Yu; Acta Crystallographica Section E 59 (2003) m977–m979; doi:10.1107/S1600536803021949

data_2202824
_publ_section_title
{<i>N,N</i>'-Bis[3-methoxymethyl-5-methylsalicylidene]-(<i>R,R</i>)-1,2-diphenylenediamino}nickel(II)
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m977
_journal_page_last               m979
_journal_paper_doi               10.1107/S1600536803021949
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C34 H34 N2 O4)]'
_chemical_formula_moiety         'C34 H34 N2 Ni O4'
_chemical_formula_sum            'C34 H34 N2 Ni O4'
_chemical_formula_weight         593.34
_chemical_melting_point          512
_chemical_name_common
;
{N,N'-Bis[3-methoxymethyl-5-methylsalicylidene]-(R,R)-1,2-
diphenylenediamino}nickel(II)
;
_chemical_name_systematic
;
6,6'-bis(methoxymethyl)-4,4'-dimethyl-2,2'-[1,2-diphenyl-1,2-
ethanediylbis(nitrilomethylidyne)]diphenol
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.101(3)
_cell_length_b                   13.7600(10)
_cell_length_c                   8.9890(10)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14.18
_cell_measurement_theta_min      2.98
_cell_volume                     2927.5(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1996)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7965
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        2.53
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL; Siemens, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.272
_refine_ls_abs_structure_details 'Flack (1983), 3473 Friedel pairs'
_refine_ls_abs_structure_Flack   0.038(15)
_refine_ls_extinction_coef       0.00045(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0454P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                5073
_reflns_number_total             7242
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6309.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2927.3(5)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2202824
_cod_database_fobs_code          2202824