{6,6'-Dimethoxy-2,2'-[(cyclohexane-1,2-diyl)bis(nitriliomethylidyne)]diphenolato}trinitratolanthanum(III) methanol monosolvate
Chen, Peng; Bao, Yan; Yan, Peng-Fei; Li, Guang-Ming; Acta Crystallographica Section E 66 (2010) m1177–; doi:10.1107/S1600536810033453

data_2228040
_publ_section_title
;
 {6,6'-Dimethoxy-2,2'-[(cyclohexane-1,2-diyl)bis(nitriliomethylidyne)]diphenolato}trinitratolanthanum(III)
 methanol monosolvate
;
_journal_coeditor_code           VM2037
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1177
_journal_paper_doi               10.1107/S1600536810033453
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[La (N O3)3 (C22 H26 N2 O4)], C H4 O'
_chemical_formula_moiety         'C22 H26 La N5 O13, C H4 O'
_chemical_formula_sum            'C23 H30 La N5 O14'
_chemical_formula_weight         739.43
_chemical_name_systematic
;
{6,6'-Dimethoxy-2,2'-[(cyclohexane-1,2-
diyl)bis(nitriliomethylidyne)]diphenolato}trinitratolanthanum(III) methanol
monosolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                79.3740(10)
_cell_angle_beta                 68.7430(10)
_cell_angle_gamma                82.2700(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7809(4)
_cell_length_b                   12.8783(5)
_cell_length_c                   13.0904(5)
_cell_measurement_reflns_used    6687
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.66
_cell_volume                     1506.22(10)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scan'
_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  0.0101
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10874
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.7963
_exptl_absorpt_correction_T_min  0.7253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.769
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7145
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+1.3148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                6526
_reflns_number_total             7145
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            vm2037.cif
_cod_data_source_block           I
_cod_database_code               2228040
_cod_database_fobs_code          2228040