#------------------------------------------------------------------------------
#$Date: 2021-12-13 09:59:21 +0100 (lun 13 de dic de 2021) $
#$Revision: 271352 $
#$URL: svn://www.crystallography.net/cod/cif/1/56/56/1565678.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1565678
loop_
_publ_author_name
'Banerjee, Saikat'
'Ghorai, Pravat'
'Sarkar, Papiya'
'Panja, Anangamohan'
'Saha, Amrita'
_publ_section_title
;
 A rare flattened tetrahedral Mn(II) salen type complex: Synthesis,
 crystal structure, biomimetic catalysis and DFT study
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119176
_journal_paper_doi               10.1016/j.ica.2019.119176
_journal_volume                  499
_journal_year                    2020
_chemical_formula_sum            'C19 H20 Mn N2 O4'
_chemical_formula_weight         395.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7944(10)
_cell_length_b                   8.0362(3)
_cell_length_c                   8.6956(4)
_cell_measurement_reflns_used    460
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      0.998
_cell_volume                     1732.62(12)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25178
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.160
_diffrn_reflns_theta_min         1.643
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       Needle
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0477
_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/[σ²(Fo²)+(0.0988P)²+1.1070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1520
_reflns_number_total             1926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-499-119176.cif
_cod_data_source_block           1
_cod_database_code               1565678
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.927
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
'x-1/2, y-1/2, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.000000 0.02670(7) 0.750000 0.0318(2) Uani 1 2 d S T P . .
O1 O 0.12493(12) 0.4244(4) 0.7113(4) 0.0728(8) Uani 1 1 d . . . . .
O2 O 0.05582(10) 0.1889(3) 0.7656(2) 0.0526(6) Uani 1 1 d . . . . .
C4 C 0.21010(13) 0.1380(5) 0.9362(5) 0.0655(10) Uani 1 1 d . . . . .
H4 H 0.244775 0.130530 0.976393 0.079 Uiso 1 1 calc R U . . .
C3 C 0.19482(13) 0.2766(4) 0.8501(4) 0.0595(8) Uani 1 1 d . . . . .
H3 H 0.219886 0.359719 0.829399 0.071 Uiso 1 1 calc R U . . .
C9 C 0.01017(14) -0.2962(4) 0.8944(5) 0.0603(9) Uani 1 1 d . . . . .
H9A H -0.024134 -0.270133 0.942368 0.072 Uiso 1 1 calc R U . . .
H9B H 0.030771 -0.363291 0.966206 0.072 Uiso 1 1 calc R U . . .
C10 C 0.000000 -0.3965(7) 0.750000 0.0602(13) Uani 1 2 d S T P . .
H10A H 0.030922 -0.467956 0.732303 0.072 Uiso 0.5 1 calc R U P . .
H10B H -0.030920 -0.467962 0.767696 0.072 Uiso 0.5 1 calc R U P . .
C8 C 0.08680(12) -0.1209(4) 0.9220(3) 0.0490(7) Uani 1 1 d . . . . .
H8 H 0.099977 -0.206640 0.983257 0.059 Uiso 1 1 calc R U . . .
C2 C 0.14339(13) 0.2912(4) 0.7958(4) 0.0514(7) Uani 1 1 d . . . . .
N1 N 0.03958(10) -0.1401(3) 0.8646(3) 0.0489(6) Uani 1 1 d . . . . .
C1 C 0.15788(18) 0.5673(5) 0.7067(6) 0.0731(10) Uani 1 1 d . . . . .
H1A H 0.162926 0.609002 0.809092 0.110 Uiso 1 1 calc R U . . .
H1B H 0.140905 0.651068 0.644629 0.110 Uiso 1 1 calc R U . . .
H1C H 0.192256 0.539020 0.663061 0.110 Uiso 1 1 calc R U . . .
C5 C 0.17349(15) 0.0129(4) 0.9612(5) 0.0603(9) Uani 1 1 d . . . . .
H5 H 0.183583 -0.078952 1.019484 0.072 Uiso 1 1 calc R U . . .
C7 C 0.10417(11) 0.1647(4) 0.8191(3) 0.0453(7) Uani 1 1 d . . . . .
C6 C 0.12115(12) 0.0209(4) 0.9005(4) 0.0482(7) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Mn O2 93.70(15) . 3_556
O2 Mn N1 151.36(10) . 3_556
O2 Mn N1 93.95(10) 3_556 3_556
O2 Mn N1 93.95(10) . .
O2 Mn N1 151.36(10) 3_556 .
N1 Mn N1 92.42(15) 3_556 .
C2 O1 C1 117.1(3) . .
C7 O2 Mn 126.3(2) . .
C5 C4 C3 119.4(3) . .
C5 C4 H4 120.3 . .
C3 C4 H4 120.3 . .
C2 C3 C4 120.6(3) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
N1 C9 C10 112.9(3) . .
N1 C9 H9A 109.0 . .
C10 C9 H9A 109.0 . .
N1 C9 H9B 109.0 . .
C10 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C9 C10 C9 115.6(4) 3_556 .
C9 C10 H10A 108.4 3_556 .
C9 C10 H10A 108.4 . .
C9 C10 H10B 108.4 3_556 .
C9 C10 H10B 108.4 . .
H10A C10 H10B 107.4 . .
N1 C8 C6 125.9(3) . .
N1 C8 H8 117.0 . .
C6 C8 H8 117.0 . .
C3 C2 O1 124.2(3) . .
C3 C2 C7 121.9(3) . .
O1 C2 C7 113.9(3) . .
C8 N1 C9 119.1(3) . .
C8 N1 Mn 125.4(2) . .
C9 N1 Mn 115.4(2) . .
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C4 C5 C6 121.3(3) . .
C4 C5 H5 119.4 . .
C6 C5 H5 119.4 . .
O2 C7 C6 125.0(3) . .
O2 C7 C2 118.2(3) . .
C6 C7 C2 116.8(3) . .
C5 C6 C7 119.9(3) . .
C5 C6 C8 117.7(3) . .
C7 C6 C8 122.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn O2 1.906(2) .
Mn O2 1.906(2) 3_556
Mn N1 1.937(2) 3_556
Mn N1 1.937(2) .
O1 C2 1.376(4) .
O1 C1 1.410(4) .
O2 C7 1.301(4) .
C4 C5 1.372(5) .
C4 C3 1.395(5) .
C4 H4 0.9300 .
C3 C2 1.365(5) .
C3 H3 0.9300 .
C9 N1 1.474(4) .
C9 C10 1.514(5) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C8 N1 1.282(4) .
C8 C6 1.435(4) .
C8 H8 0.9300 .
C2 C7 1.422(4) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C5 C6 1.402(5) .
C5 H5 0.9300 .
C7 C6 1.419(4) .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{5e335088-0d3e-4653-bfa4-cdb96fe8e815} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{5e335088-0d3e-4653-bfa4-cdb96fe8e815} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
EE
