#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:57:14 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268835 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/07/7060739.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_7060739
loop_
_publ_author_name
'Bortoluzzi, Marco'
'Castro, Jesús'
'Di Vera, Andrea'
'Palù, Alberto'
'Ferraro, Valentina'
_publ_section_title
;
 Manganese(ii) bromo- and iodo-complexes with phosphoramidate and
 phosphonate ligands: synthesis, characterization and photoluminescence
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12871
_journal_page_last               12878
_journal_paper_doi               10.1039/D1NJ02053F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C14 H28 I2 Mn N4 O4 P2'
_chemical_formula_weight         687.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-11-17 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.395(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1151(9)
_cell_length_b                   14.0317(12)
_cell_length_c                   16.0386(14)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.45
_cell_volume                     2460.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_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 1.000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50220
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.345
_diffrn_reflns_theta_min         2.362
_exptl_absorpt_coefficient_mu    3.201
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       prism
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.205
_refine_diff_density_max         1.946
_refine_diff_density_min         -2.470
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0395
_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)+(0.0325P)²+16.5353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5510
_reflns_number_total             6143
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj02053f2.cif
_cod_data_source_block           MnI2_mu[O=P(NMe2]2)Ph
_cod_depositor_comments
'Adding full bibliography for 7060738--7060741.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7060739
_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   0.484
_shelx_estimated_absorpt_t_max   0.560
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.00984(5) 0.33487(4) 0.75724(4) 0.01389(13) Uani 1 1 d . . . . .
I1 I -0.14997(3) 0.47561(2) 0.76506(2) 0.02514(9) Uani 1 1 d . . . . .
I2 I -0.04059(3) 0.22922(2) 0.61845(2) 0.03035(9) Uani 1 1 d . . . . .
P1 P 0.31220(10) 0.36099(8) 0.76919(7) 0.0152(2) Uani 1 1 d . . . . .
O11 O 0.1813(3) 0.3883(2) 0.76278(19) 0.0188(6) Uani 1 1 d . . . . .
O12 O 0.4615(3) 0.7551(2) 0.63497(19) 0.0197(6) Uani 1 1 d . . . . .
N11 N 0.3962(3) 0.4365(3) 0.8301(2) 0.0221(8) Uani 1 1 d . . . . .
N12 N 0.3527(4) 0.2528(3) 0.7978(2) 0.0218(8) Uani 1 1 d . . . . .
C11 C 0.5300(4) 0.4315(4) 0.8415(4) 0.0373(13) Uani 1 1 d . . . . .
H11A H 0.563142 0.495542 0.836667 0.056 Uiso 1 1 calc R U . . .
H11B H 0.553403 0.390218 0.797750 0.056 Uiso 1 1 calc R U . . .
H11C H 0.562807 0.405285 0.897623 0.056 Uiso 1 1 calc R U . . .
C12 C 0.3491(5) 0.4936(4) 0.8937(3) 0.0288(10) Uani 1 1 d . . . . .
H12A H 0.370976 0.463114 0.949291 0.043 Uiso 1 1 calc R U . . .
H12B H 0.259919 0.498393 0.878197 0.043 Uiso 1 1 calc R U . . .
H12C H 0.385003 0.557585 0.895967 0.043 Uiso 1 1 calc R U . . .
C13 C 0.3088(5) 0.1710(3) 0.7438(4) 0.0314(11) Uani 1 1 d . . . . .
H13A H 0.370797 0.120598 0.752126 0.047 Uiso 1 1 calc R U . . .
H13B H 0.293469 0.190948 0.684235 0.047 Uiso 1 1 calc R U . . .
H13C H 0.232808 0.146950 0.758897 0.047 Uiso 1 1 calc R U . . .
C14 C 0.3765(5) 0.2294(4) 0.8886(3) 0.0362(12) Uani 1 1 d . . . . .
H14A H 0.300444 0.208120 0.905585 0.054 Uiso 1 1 calc R U . . .
H14B H 0.407261 0.286053 0.921373 0.054 Uiso 1 1 calc R U . . .
H14C H 0.437579 0.178420 0.899435 0.054 Uiso 1 1 calc R U . . .
C1 C 0.3250(4) 0.4362(3) 0.6204(3) 0.0167(8) Uani 1 1 d . . . . .
C2 C 0.4186(4) 0.5000(3) 0.6123(3) 0.0156(8) Uani 1 1 d . . . . .
H2 H 0.495044 0.498270 0.649938 0.019 Uiso 1 1 calc R U . . .
C3 C 0.3955(4) 0.5656(3) 0.5473(3) 0.0154(8) Uani 1 1 d . . . . .
C4 C 0.2846(4) 0.5704(3) 0.4926(3) 0.0203(8) Uani 1 1 d . . . . .
H4 H 0.271331 0.615839 0.447941 0.024 Uiso 1 1 calc R U . . .
C5 C 0.1928(4) 0.5073(3) 0.5042(3) 0.0234(9) Uani 1 1 d . . . . .
H5 H 0.115479 0.510600 0.467693 0.028 Uiso 1 1 calc R U . . .
C6 C 0.2119(4) 0.4393(3) 0.5683(3) 0.0204(9) Uani 1 1 d . . . . .
H6 H 0.148862 0.396192 0.575921 0.024 Uiso 1 1 calc R U . . .
P2 P 0.50334(9) 0.73390(7) 0.55345(6) 0.0135(2) Uani 1 1 d . . . . .
O21 O 0.4945(3) 0.6231(2) 0.53430(18) 0.0154(6) Uani 1 1 d . . . . .
O22 O 0.3532(3) 0.3621(2) 0.6794(2) 0.0204(6) Uani 1 1 d . . . . .
N21 N 0.4190(3) 0.7884(2) 0.4750(2) 0.0158(7) Uani 1 1 d . . . . .
N22 N 0.6468(3) 0.7527(3) 0.5523(3) 0.0213(8) Uani 1 1 d . . . . .
C21 C 0.4178(4) 0.7613(3) 0.3864(3) 0.0217(9) Uani 1 1 d . . . . .
H21A H 0.333082 0.757939 0.355970 0.033 Uiso 1 1 calc R U . . .
H21B H 0.456778 0.698829 0.384567 0.033 Uiso 1 1 calc R U . . .
H21C H 0.462707 0.808876 0.359415 0.033 Uiso 1 1 calc R U . . .
C22 C 0.6906(5) 0.8350(4) 0.5115(3) 0.0296(11) Uani 1 1 d . . . . .
H22A H 0.715335 0.885053 0.553665 0.044 Uiso 1 1 calc R U . . .
H22B H 0.625166 0.858888 0.467195 0.044 Uiso 1 1 calc R U . . .
H22C H 0.760964 0.816363 0.486041 0.044 Uiso 1 1 calc R U . . .
C23 C 0.7389(5) 0.7077(4) 0.6183(4) 0.0335(12) Uani 1 1 d . . . . .
H23A H 0.809805 0.688607 0.593682 0.050 Uiso 1 1 calc R U . . .
H23B H 0.703313 0.651432 0.640607 0.050 Uiso 1 1 calc R U . . .
H23C H 0.764828 0.753294 0.664303 0.050 Uiso 1 1 calc R U . . .
C24 C 0.3662(5) 0.8819(3) 0.4870(3) 0.0320(11) Uani 1 1 d . . . . .
H24A H 0.412731 0.931410 0.463639 0.048 Uiso 1 1 calc R U . . .
H24B H 0.369723 0.893409 0.547656 0.048 Uiso 1 1 calc R U . . .
H24C H 0.280825 0.883466 0.457746 0.048 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
O11 Mn O12 99.42(13) . 2_546 ?
O11 Mn I2 107.30(9) . . ?
O12 Mn I2 112.50(9) 2_546 . ?
O11 Mn I1 110.52(9) . . ?
O12 Mn I1 111.71(9) 2_546 . ?
I2 Mn I1 114.27(2) . . ?
O11 P1 O22 111.80(18) . . ?
O11 P1 N11 108.85(19) . . ?
O22 P1 N11 108.21(19) . . ?
O11 P1 N12 118.48(19) . . ?
O22 P1 N12 98.91(18) . . ?
N11 P1 N12 109.9(2) . . ?
P1 O11 Mn 143.4(2) . . ?
P2 O12 Mn 145.7(2) . 2_556 ?
C12 N11 C11 114.9(4) . . ?
C12 N11 P1 122.6(3) . . ?
C11 N11 P1 120.4(3) . . ?
C13 N12 C14 113.1(4) . . ?
C13 N12 P1 121.2(3) . . ?
C14 N12 P1 118.6(4) . . ?
C6 C1 C2 122.4(4) . . ?
C6 C1 O22 120.0(4) . . ?
C2 C1 O22 117.4(4) . . ?
C3 C2 C1 117.3(4) . . ?
C2 C3 C4 122.4(4) . . ?
C2 C3 O21 116.8(4) . . ?
C4 C3 O21 120.6(4) . . ?
C3 C4 C5 118.5(4) . . ?
C4 C5 C6 121.3(4) . . ?
C1 C6 C5 118.1(4) . . ?
O12 P2 O21 110.26(17) . . ?
O12 P2 N21 110.97(18) . . ?
O21 P2 N21 107.80(17) . . ?
O12 P2 N22 116.1(2) . . ?
O21 P2 N22 100.62(18) . . ?
N21 P2 N22 110.36(19) . . ?
C3 O21 P2 123.8(2) . . ?
C1 O22 P1 123.6(3) . . ?
C24 N21 C21 115.2(4) . . ?
C24 N21 P2 120.7(3) . . ?
C21 N21 P2 122.1(3) . . ?
C22 N22 C23 114.7(4) . . ?
C22 N22 P2 123.0(3) . . ?
C23 N22 P2 118.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn O11 2.035(3) . ?
Mn O12 2.036(3) 2_546 ?
Mn I2 2.6489(7) . ?
Mn I1 2.6742(7) . ?
P1 O11 1.490(3) . ?
P1 O22 1.587(3) . ?
P1 N11 1.618(4) . ?
P1 N12 1.626(4) . ?
O12 P2 1.495(3) . ?
N11 C12 1.466(6) . ?
N11 C11 1.467(6) . ?
N12 C13 1.466(6) . ?
N12 C14 1.470(6) . ?
C1 C6 1.380(6) . ?
C1 C2 1.396(6) . ?
C1 O22 1.403(5) . ?
C2 C3 1.379(6) . ?
C3 C4 1.380(6) . ?
C3 O21 1.409(5) . ?
C4 C5 1.389(6) . ?
C5 C6 1.390(6) . ?
P2 O21 1.585(3) . ?
P2 N21 1.620(4) . ?
P2 N22 1.620(4) . ?
N21 C24 1.464(6) . ?
N21 C21 1.469(5) . ?
N22 C22 1.454(6) . ?
N22 C23 1.474(6) . ?
