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#$Date: 2020-10-06 13:07:50 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257751 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/91/7059184.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_7059184
loop_
_publ_author_name
'Bortoluzzi, Marco'
'Castro, Jesús'
'Gobbo, Alberto'
'Ferraro, Valentina'
'Pietrobon, Luca'
'Antoniutti, Stefano'
_publ_section_title
;
 Tetrahedral photoluminescent manganese(ii) halide complexes with
 1,3-dimethyl-2-phenyl-1,3-diazaphospholidine-2-oxide as a ligand
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              571
_journal_page_last               579
_journal_paper_doi               10.1039/C9NJ05083C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C20 H30 Cl2 Mn N4 O2 P2'
_chemical_formula_weight         546.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-27 deposited with the CCDC.	2019-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.687(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4104(6)
_cell_length_b                   13.4995(6)
_cell_length_c                   14.4145(7)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.41
_cell_volume                     2545.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_source         'Incoatec high brillance I\muS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.791
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+2.3663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2716
_reflns_number_total             3182
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj05083c3.cif
_cod_data_source_block           32043403_0m_a
_cod_depositor_comments
'Adding full bibliography for 7059184--7059185.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7059184
_shelx_shelxl_version_number     2018/3
_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   0.808
_shelx_estimated_absorpt_t_max   0.867
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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
Mn1 Mn 0.500000 0.70686(2) 0.750000 0.01200(9) Uani 1 2 d S T P
Cl1 Cl 0.54067(3) 0.79343(3) 0.62274(3) 0.02978(12) Uani 1 1 d . . .
P1 P 0.28761(3) 0.55555(3) 0.69645(3) 0.01120(9) Uani 1 1 d . . .
O1 O 0.38317(8) 0.61203(7) 0.69419(7) 0.0139(2) Uani 1 1 d . . .
C11 C 0.31590(11) 0.47145(10) 0.79504(10) 0.0124(3) Uani 1 1 d . . .
C12 C 0.23728(12) 0.40961(11) 0.81039(11) 0.0164(3) Uani 1 1 d . . .
H12 H 0.171410 0.413460 0.769439 0.020 Uiso 1 1 calc R U .
C13 C 0.25536(13) 0.34276(11) 0.88522(11) 0.0187(3) Uani 1 1 d . . .
H13 H 0.201865 0.300905 0.895505 0.022 Uiso 1 1 calc R U .
C14 C 0.35142(13) 0.33693(11) 0.94505(11) 0.0189(3) Uani 1 1 d . . .
H14 H 0.363652 0.290983 0.996223 0.023 Uiso 1 1 calc R U .
C15 C 0.42973(12) 0.39798(12) 0.93043(11) 0.0192(3) Uani 1 1 d . . .
H15 H 0.495426 0.393764 0.971653 0.023 Uiso 1 1 calc R U .
C16 C 0.41237(12) 0.46539(11) 0.85558(10) 0.0165(3) Uani 1 1 d . . .
H16 H 0.466084 0.507193 0.845721 0.020 Uiso 1 1 calc R U .
N1 N 0.23323(9) 0.49398(9) 0.60175(9) 0.0159(3) Uani 1 1 d . . .
N2 N 0.18682(10) 0.62408(9) 0.69807(10) 0.0177(3) Uani 1 1 d . . .
C1 C 0.28228(13) 0.41914(11) 0.55483(11) 0.0203(3) Uani 1 1 d . . .
H1A H 0.237651 0.361066 0.540907 0.030 Uiso 1 1 calc R U .
H1B H 0.347326 0.399762 0.596541 0.030 Uiso 1 1 calc R U .
H1C H 0.295001 0.446061 0.495349 0.030 Uiso 1 1 calc R U .
C2 C 0.13178(12) 0.53055(12) 0.55608(11) 0.0207(3) Uani 1 1 d . . .
H2A H 0.085178 0.474725 0.532591 0.025 Uiso 1 1 calc R U .
H2B H 0.135623 0.574219 0.501799 0.025 Uiso 1 1 calc R U .
C3 C 0.09430(12) 0.58814(13) 0.63280(12) 0.0225(3) Uani 1 1 d . . .
H3A H 0.050509 0.644287 0.604564 0.027 Uiso 1 1 calc R U .
H3B H 0.054545 0.544598 0.666540 0.027 Uiso 1 1 calc R U .
C4 C 0.17560(14) 0.68163(13) 0.78044(13) 0.0259(4) Uani 1 1 d . . .
H4A H 0.135188 0.741175 0.759269 0.039 Uiso 1 1 calc R U .
H4B H 0.243272 0.700921 0.817149 0.039 Uiso 1 1 calc R U .
H4C H 0.140793 0.641573 0.820406 0.039 Uiso 1 1 calc R U .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1 Mn1 O1 102.55(6) 2_656 .
O1 Mn1 Cl1 109.31(3) 2_656 .
O1 Mn1 Cl1 107.13(3) . .
O1 Mn1 Cl1 107.13(3) 2_656 2_656
O1 Mn1 Cl1 109.31(3) . 2_656
Cl1 Mn1 Cl1 120.03(3) . 2_656
O1 P1 N1 118.01(6) . .
O1 P1 N2 115.11(6) . .
N1 P1 N2 94.65(7) . .
O1 P1 C11 107.85(6) . .
N1 P1 C11 108.61(7) . .
N2 P1 C11 112.15(7) . .
P1 O1 Mn1 153.49(7) . .
C16 C11 C12 119.55(13) . .
C16 C11 P1 122.59(11) . .
C12 C11 P1 117.86(11) . .
C13 C12 C11 120.14(14) . .
C14 C13 C12 120.05(14) . .
C13 C14 C15 120.19(14) . .
C14 C15 C16 120.20(15) . .
C15 C16 C11 119.85(14) . .
C1 N1 C2 119.85(13) . .
C1 N1 P1 125.52(11) . .
C2 N1 P1 114.00(11) . .
C4 N2 C3 118.44(13) . .
C4 N2 P1 123.07(11) . .
C3 N2 P1 112.82(11) . .
N1 C2 C3 105.56(12) . .
N2 C3 C2 105.49(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.0462(10) 2_656
Mn1 O1 2.0463(10) .
Mn1 Cl1 2.3383(4) .
Mn1 Cl1 2.3384(4) 2_656
P1 O1 1.4977(10) .
P1 N1 1.6275(13) .
P1 N2 1.6422(13) .
P1 C11 1.7932(14) .
C11 C16 1.395(2) .
C11 C12 1.400(2) .
C12 C13 1.386(2) .
C13 C14 1.386(2) .
C14 C15 1.387(2) .
C15 C16 1.392(2) .
N1 C1 1.451(2) .
N1 C2 1.4610(19) .
N2 C4 1.454(2) .
N2 C3 1.465(2) .
C2 C3 1.524(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 P1 O1 Mn1 174.68(13)
N2 P1 O1 Mn1 64.15(16)
C11 P1 O1 Mn1 -61.88(16)
O1 P1 C11 C16 0.34(14)
N1 P1 C11 C16 129.32(13)
N2 P1 C11 C16 -127.42(13)
O1 P1 C11 C12 -179.27(11)
N1 P1 C11 C12 -50.29(13)
N2 P1 C11 C12 52.97(13)
C16 C11 C12 C13 -0.1(2)
P1 C11 C12 C13 179.54(12)
C11 C12 C13 C14 0.0(2)
C12 C13 C14 C15 0.1(2)
C13 C14 C15 C16 -0.1(2)
C14 C15 C16 C11 -0.1(2)
C12 C11 C16 C15 0.1(2)
P1 C11 C16 C15 -179.47(12)
O1 P1 N1 C1 55.58(14)
N2 P1 N1 C1 177.28(13)
C11 P1 N1 C1 -67.47(14)
O1 P1 N1 C2 -115.23(11)
N2 P1 N1 C2 6.47(11)
C11 P1 N1 C2 121.72(11)
O1 P1 N2 C4 -71.30(14)
N1 P1 N2 C4 164.75(13)
C11 P1 N2 C4 52.49(14)
O1 P1 N2 C3 135.76(11)
N1 P1 N2 C3 11.81(12)
C11 P1 N2 C3 -100.45(11)
C1 N1 C2 C3 167.25(13)
P1 N1 C2 C3 -21.37(15)
C4 N2 C3 C2 -179.37(13)
P1 N2 C3 C2 -25.07(15)
N1 C2 C3 N2 27.65(16)
