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#$Date: 2020-07-06 06:02:16 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253883 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/44/7704484.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_7704484
loop_
_publ_author_name
'Bortoluzzi, Marco'
'Castro, Jesús'
'Gobbo, Alberto'
'Ferraro, Valentina'
'Pietrobon, Luca'
_publ_section_title
;
 Light harvesting indolyl-substituted phosphoramide ligand for the
 enhancement of Mn(ii) luminescence.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7525
_journal_page_last               7534
_journal_paper_doi               10.1039/d0dt01659d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H36 I2 Mn N6 O2 P2'
_chemical_formula_sum            'C24 H36 I2 Mn N6 O2 P2'
_chemical_formula_weight         811.27
_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     'SHELXT 2018/2 (Sheldrick, 2018)'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-12-20 deposited with the CCDC.	2020-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.640(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6662(7)
_cell_length_b                   15.8451(12)
_cell_length_c                   19.6427(15)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.33
_cell_volume                     3262.7(4)
_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  'SHELXL-2018/3 (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 0.998
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56685
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.377
_diffrn_reflns_theta_min         2.330
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       prism
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.169
_refine_diff_density_max         0.742
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         8153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0178P)²+3.6657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7437
_reflns_number_total             8153
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01659d3.cif
_cod_data_source_block           32061203_0m_a
_cod_depositor_comments
'Adding full bibliography for 7704484--7704486.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704484
_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   0.600
_shelx_estimated_absorpt_t_max   0.685
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 0.70324(3) 0.76013(2) 0.39503(2) 0.01071(6) Uani 1 1 d . . . . .
I1 I 0.93714(2) 0.80489(2) 0.37747(2) 0.01954(4) Uani 1 1 d . . . . .
I2 I 0.51041(2) 0.84950(2) 0.32439(2) 0.02026(4) Uani 1 1 d . . . . .
P1 P 0.64332(5) 0.54591(3) 0.36022(3) 0.01170(10) Uani 1 1 d . . . . .
O1 O 0.65952(14) 0.63866(9) 0.36902(8) 0.0174(3) Uani 1 1 d . . . . .
N11 N 0.49688(15) 0.52548(10) 0.31501(8) 0.0131(3) Uani 1 1 d . . . . .
C12 C 0.4670(2) 0.45531(13) 0.27091(10) 0.0159(4) Uani 1 1 d . . . . .
H12 H 0.527631 0.422380 0.252788 0.019 Uiso 1 1 calc R U . . .
C13 C 0.3405(2) 0.44163(13) 0.25816(11) 0.0175(4) Uani 1 1 d . . . . .
H13 H 0.297110 0.398300 0.229716 0.021 Uiso 1 1 calc R U . . .
C14 C 0.15589(19) 0.52187(13) 0.30183(11) 0.0182(4) Uani 1 1 d . . . . .
H14 H 0.087718 0.487707 0.279004 0.022 Uiso 1 1 calc R U . . .
C15 C 0.13277(19) 0.58966(13) 0.34205(11) 0.0181(4) Uani 1 1 d . . . . .
H15 H 0.047663 0.602043 0.346794 0.022 Uiso 1 1 calc R U . . .
C16 C 0.2323(2) 0.64024(13) 0.37584(11) 0.0172(4) Uani 1 1 d . . . . .
H16 H 0.213432 0.686580 0.402945 0.021 Uiso 1 1 calc R U . . .
C17 C 0.35793(19) 0.62436(12) 0.37072(10) 0.0148(4) Uani 1 1 d . . . . .
H17 H 0.425494 0.658902 0.393701 0.018 Uiso 1 1 calc R U . . .
C18 C 0.38120(18) 0.55588(12) 0.33061(10) 0.0122(4) Uani 1 1 d . . . . .
C19 C 0.28250(19) 0.50458(12) 0.29543(10) 0.0141(4) Uani 1 1 d . . . . .
N12 N 0.74545(16) 0.50736(11) 0.31667(9) 0.0152(3) Uani 1 1 d . . . . .
C121 C 0.7668(2) 0.54954(15) 0.25350(12) 0.0236(5) Uani 1 1 d . . . . .
H12A H 0.858510 0.552118 0.253331 0.035 Uiso 1 1 calc R U . . .
H12B H 0.732014 0.606910 0.251913 0.035 Uiso 1 1 calc R U . . .
H12C H 0.724051 0.517837 0.212945 0.035 Uiso 1 1 calc R U . . .
C122 C 0.7981(2) 0.42260(15) 0.32620(14) 0.0294(5) Uani 1 1 d . . . . .
H12D H 0.760613 0.387310 0.286694 0.044 Uiso 1 1 calc R U . . .
H12E H 0.778426 0.398353 0.368904 0.044 Uiso 1 1 calc R U . . .
H12F H 0.890853 0.425028 0.329434 0.044 Uiso 1 1 calc R U . . .
N13 N 0.65164(16) 0.49712(11) 0.43355(9) 0.0158(3) Uani 1 1 d . . . . .
C131 C 0.7578(2) 0.51638(16) 0.49013(13) 0.0299(5) Uani 1 1 d . . . . .
H13A H 0.725383 0.522929 0.533392 0.045 Uiso 1 1 calc R U . . .
H13B H 0.799017 0.568904 0.479799 0.045 Uiso 1 1 calc R U . . .
H13C H 0.819900 0.470198 0.495076 0.045 Uiso 1 1 calc R U . . .
C132 C 0.5810(2) 0.42038(14) 0.44396(11) 0.0210(4) Uani 1 1 d . . . . .
H13D H 0.639579 0.372203 0.450653 0.031 Uiso 1 1 calc R U . . .
H13E H 0.514315 0.410467 0.403222 0.031 Uiso 1 1 calc R U . . .
H13F H 0.541727 0.427114 0.484986 0.031 Uiso 1 1 calc R U . . .
P2 P 0.72007(5) 0.81790(3) 0.56343(3) 0.01224(10) Uani 1 1 d . . . . .
O2 O 0.70092(13) 0.76688(9) 0.49831(7) 0.0148(3) Uani 1 1 d . . . . .
N21 N 0.60271(16) 0.79457(11) 0.60636(9) 0.0144(3) Uani 1 1 d . . . . .
C22 C 0.6159(2) 0.78264(14) 0.67823(10) 0.0186(4) Uani 1 1 d . . . . .
H22 H 0.695093 0.778268 0.709439 0.022 Uiso 1 1 calc R U . . .
C23 C 0.5005(2) 0.77826(14) 0.69663(11) 0.0209(4) Uani 1 1 d . . . . .
H23 H 0.484599 0.769570 0.742124 0.025 Uiso 1 1 calc R U . . .
C24 C 0.2719(2) 0.79082(13) 0.62149(12) 0.0208(4) Uani 1 1 d . . . . .
H24 H 0.225318 0.782767 0.657793 0.025 Uiso 1 1 calc R U . . .
C25 C 0.2094(2) 0.80442(13) 0.55457(13) 0.0216(5) Uani 1 1 d . . . . .
H25 H 0.118811 0.805729 0.544929 0.026 Uiso 1 1 calc R U . . .
C26 C 0.2767(2) 0.81640(13) 0.50023(12) 0.0191(4) Uani 1 1 d . . . . .
H26 H 0.230828 0.826358 0.454707 0.023 Uiso 1 1 calc R U . . .
C27 C 0.4085(2) 0.81396(12) 0.51182(11) 0.0154(4) Uani 1 1 d . . . . .
H27 H 0.454366 0.821635 0.475150 0.018 Uiso 1 1 calc R U . . .
C28 C 0.47124(19) 0.79976(12) 0.57953(10) 0.0137(4) Uani 1 1 d . . . . .
C29 C 0.4060(2) 0.78909(12) 0.63506(11) 0.0164(4) Uani 1 1 d . . . . .
N22 N 0.85511(17) 0.79361(11) 0.61193(9) 0.0174(4) Uani 1 1 d . . . . .
C221 C 0.9243(2) 0.84980(15) 0.66517(13) 0.0269(5) Uani 1 1 d . . . . .
H22A H 0.930155 0.823486 0.710807 0.040 Uiso 1 1 calc R U . . .
H22B H 0.878627 0.903581 0.664325 0.040 Uiso 1 1 calc R U . . .
H22C H 1.010259 0.859921 0.656018 0.040 Uiso 1 1 calc R U . . .
C222 C 0.9034(2) 0.70675(14) 0.61460(13) 0.0249(5) Uani 1 1 d . . . . .
H22D H 0.992666 0.707066 0.608668 0.037 Uiso 1 1 calc R U . . .
H22E H 0.852296 0.673553 0.577415 0.037 Uiso 1 1 calc R U . . .
H22F H 0.897608 0.681602 0.659488 0.037 Uiso 1 1 calc R U . . .
N23 N 0.71129(18) 0.91883(11) 0.55221(10) 0.0191(4) Uani 1 1 d . . . . .
C231 C 0.6418(2) 0.97833(13) 0.58842(11) 0.0203(4) Uani 1 1 d . . . . .
H23A H 0.701948 1.018372 0.614807 0.030 Uiso 1 1 calc R U . . .
H23B H 0.597507 0.947357 0.620128 0.030 Uiso 1 1 calc R U . . .
H23C H 0.579305 1.009116 0.554573 0.030 Uiso 1 1 calc R U . . .
C232 C 0.7929(3) 0.95933(15) 0.50896(15) 0.0376(7) Uani 1 1 d . . . . .
H23D H 0.740216 0.994204 0.473549 0.056 Uiso 1 1 calc R U . . .
H23E H 0.836361 0.915858 0.486478 0.056 Uiso 1 1 calc R U . . .
H23F H 0.856391 0.994915 0.538050 0.056 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
O1 Mn O2 104.88(6) . . ?
O1 Mn I2 104.72(4) . . ?
O2 Mn I2 109.91(4) . . ?
O1 Mn I1 113.35(4) . . ?
O2 Mn I1 107.31(4) . . ?
I2 Mn I1 116.111(12) . . ?
O1 P1 N13 112.45(9) . . ?
O1 P1 N12 110.99(9) . . ?
N13 P1 N12 110.88(9) . . ?
O1 P1 N11 109.20(8) . . ?
N13 P1 N11 105.71(9) . . ?
N12 P1 N11 107.33(9) . . ?
P1 O1 Mn 170.53(10) . . ?
C12 N11 C18 107.18(16) . . ?
C12 N11 P1 124.04(14) . . ?
C18 N11 P1 125.80(13) . . ?
C13 C12 N11 110.33(18) . . ?
C12 C13 C19 107.69(18) . . ?
C15 C14 C19 118.57(19) . . ?
C14 C15 C16 121.17(19) . . ?
C17 C16 C15 121.46(19) . . ?
C16 C17 C18 117.34(18) . . ?
C17 C18 C19 122.27(18) . . ?
C17 C18 N11 130.16(18) . . ?
C19 C18 N11 107.55(16) . . ?
C14 C19 C18 119.18(18) . . ?
C14 C19 C13 133.57(19) . . ?
C18 C19 C13 107.25(17) . . ?
C122 N12 C121 114.45(17) . . ?
C122 N12 P1 124.08(15) . . ?
C121 N12 P1 119.96(14) . . ?
C131 N13 C132 114.36(17) . . ?
C131 N13 P1 118.84(15) . . ?
C132 N13 P1 125.05(14) . . ?
O2 P2 N23 115.06(9) . . ?
O2 P2 N22 109.93(9) . . ?
N23 P2 N22 109.79(10) . . ?
O2 P2 N21 108.34(9) . . ?
N23 P2 N21 104.92(9) . . ?
N22 P2 N21 108.52(9) . . ?
P2 O2 Mn 148.86(9) . . ?
C22 N21 C28 107.01(16) . . ?
C22 N21 P2 126.15(15) . . ?
C28 N21 P2 125.78(14) . . ?
C23 C22 N21 110.44(19) . . ?
C22 C23 C29 107.60(19) . . ?
C25 C24 C29 118.7(2) . . ?
C24 C25 C26 121.4(2) . . ?
C27 C26 C25 121.2(2) . . ?
C26 C27 C28 117.14(19) . . ?
C27 C28 N21 129.59(18) . . ?
C27 C28 C29 122.72(19) . . ?
N21 C28 C29 107.68(17) . . ?
C24 C29 C28 118.8(2) . . ?
C24 C29 C23 133.9(2) . . ?
C28 C29 C23 107.26(18) . . ?
C221 N22 C222 114.67(18) . . ?
C221 N22 P2 123.46(15) . . ?
C222 N22 P2 120.82(15) . . ?
C231 N23 C232 113.99(17) . . ?
C231 N23 P2 126.44(15) . . ?
C232 N23 P2 119.03(15) . . ?
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 O1 2.0237(14) . ?
Mn O2 2.0364(14) . ?
Mn I2 2.6659(3) . ?
Mn I1 2.6765(4) . ?
P1 O1 1.4861(14) . ?
P1 N13 1.6225(17) . ?
P1 N12 1.6235(17) . ?
P1 N11 1.6796(17) . ?
N11 C12 1.409(2) . ?
N11 C18 1.410(2) . ?
C12 C13 1.343(3) . ?
C13 C19 1.443(3) . ?
C14 C15 1.382(3) . ?
C14 C19 1.406(3) . ?
C15 C16 1.396(3) . ?
C16 C17 1.385(3) . ?
C17 C18 1.390(3) . ?
C18 C19 1.406(3) . ?
N12 C122 1.455(3) . ?
N12 C121 1.464(3) . ?
N13 C131 1.465(3) . ?
N13 C132 1.465(3) . ?
P2 O2 1.4950(14) . ?
P2 N23 1.6146(18) . ?
P2 N22 1.6197(18) . ?
P2 N21 1.6747(18) . ?
N21 C22 1.405(3) . ?
N21 C28 1.406(3) . ?
C22 C23 1.347(3) . ?
C23 C29 1.434(3) . ?
C24 C25 1.376(3) . ?
C24 C29 1.406(3) . ?
C25 C26 1.405(3) . ?
C26 C27 1.383(3) . ?
C27 C28 1.392(3) . ?
C28 C29 1.408(3) . ?
N22 C221 1.465(3) . ?
N22 C222 1.467(3) . ?
N23 C231 1.462(3) . ?
N23 C232 1.471(3) . ?
