N-2-Hydroxybenzaldehyde acylhydrazone-Fe(iii) complex: synthesis, crystal structure and its efficient and selective N-methylation.
Li, Zhiyou; Wu, Lamei; Zhang, Tao; Huang, Zhengxi; Qiu, Guofu; Zhou, Zhongqiang; Jin, Longfei; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7554–7560; doi:10.1039/c4dt00121d

data_7030356
_publ_section_title
;
 N-2-Hydroxybenzaldehyde acylhydrazone-Fe(iii) complex: synthesis, crystal
 structure and its efficient and selective N-methylation.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7554
_journal_page_last               7560
_journal_paper_doi               10.1039/c4dt00121d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C37 H46 Cl Fe N6 O6'
_chemical_formula_weight         762.10
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.409(4)
_cell_angle_beta                 108.611(4)
_cell_angle_gamma                98.761(5)
_cell_formula_units_Z            2
_cell_length_a                   12.311(4)
_cell_length_b                   13.132(4)
_cell_length_c                   14.299(5)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.47
_cell_volume                     2109.0(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.1380
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14069
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.035
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7284
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1329P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2299
_reflns_number_gt                4151
_reflns_number_total             7284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00121d2.cif
_cod_data_source_block           mo_121119b_0m
_cod_original_cell_volume        2109.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7030356