Preparing Mn(III) salen-type Schiff base complexes using 1,3-oxazines obtained by Mannich condensation: Towards removing ortho-hydroxyaldehydes
Bikas, Rahman; Emami, Marzieh; Ślepokura, Katarzyna; Noshiranzadeh, Nader; New J. Chem. 41 (2017) 9710–9717; doi:10.1039/C7NJ01562C

data_7056466
_publ_section_title
;
 Preparing Mn(III) salen-type Schiff base complexes using 1,3-oxazines
 obtained by Mannich condensation: Towards removing ortho-hydroxyaldehydes
;
_journal_issue                   18
_journal_name_full               'New J. Chem.'
_journal_page_first              9710
_journal_page_last               9717
_journal_paper_doi               10.1039/C7NJ01562C
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C25 H28 Mn N3 O2 S'
_chemical_formula_sum            'C25 H28 Mn N3 O2 S'
_chemical_formula_weight         479.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-14 deposited with the CCDC.
2017-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                96.34(3)
_cell_angle_beta                 92.01(3)
_cell_angle_gamma                103.59(4)
_cell_formula_units_Z            2
_cell_length_a                   8.418(4)
_cell_length_b                   9.004(4)
_cell_length_c                   14.787(4)
_cell_measurement_reflns_used    4177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.80
_cell_measurement_theta_min      2.86
_cell_volume                     1080.6(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Kuma KM4-CCD, Sapphire2, large Be window'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12754
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3580
_reflns_number_total             5117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01562c2.cif
_cod_data_source_block           2_nos473
_cod_depositor_comments
;

2018-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C50 H36 Mn2 N6 O4 S2'
_cod_original_formula_sum        'C50 H36 Mn2 N6 O4 S2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     958.85
_cod_database_code               7056466
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.849
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              87437