Non-conventional synthesis and photophysical studies of platinum(ii) complexes with methylene bridged 2,2'-dipyridylamine derivatives.
Bulatov, Evgeny; Haukka, Matti; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3369–3379; doi:10.1039/c8dt03912g

data_7049084
_publ_section_title
;
 Non-conventional synthesis and photophysical studies of platinum(ii)
 complexes with methylene bridged 2,2'-dipyridylamine derivatives.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3369
_journal_page_last               3379
_journal_paper_doi               10.1039/c8dt03912g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C17 H14 I3 N3 Pt'
_chemical_formula_sum            'C17 H14 I3 N3 Pt'
_chemical_formula_weight         836.10
_chemical_name_systematic
2-iodobenzyldi(2-pyridyl)aminediiodoplatinum(II)
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.754(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9848(4)
_cell_length_b                   17.1114(8)
_cell_length_c                   13.3644(5)
_cell_measurement_reflns_used    8153
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.5080
_cell_measurement_theta_min      2.7590
_cell_volume                     1995.76(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 8.0053
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
  1 omega  -49.00  -17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095  -37.0000 -150.0000 32

  2 omega  -14.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095  -99.0000   60.0000 68

  3 omega    5.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095   37.0000   30.0000 87

  4 omega   36.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095  178.0000   60.0000 56

  5 omega  -20.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095    0.0000 -180.0000 92

  6 omega    3.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2095   37.0000 -120.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0006405000
_diffrn_orient_matrix_UB_12      0.0376149000
_diffrn_orient_matrix_UB_13      -0.0221420000
_diffrn_orient_matrix_UB_21      0.0796138000
_diffrn_orient_matrix_UB_22      0.0031538000
_diffrn_orient_matrix_UB_23      0.0225612000
_diffrn_orient_matrix_UB_31      0.0163057000
_diffrn_orient_matrix_UB_32      -0.0171021000
_diffrn_orient_matrix_UB_33      -0.0445874000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19229
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.752
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.675
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.228
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.783
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2288
_exptl_crystal_size_mid          0.1305
_exptl_crystal_size_min          0.0551
_refine_diff_density_max         2.035
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5606
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0443
_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/[\s^2^(Fo^2^)+(0.0089P)^2^+23.2925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4717
_reflns_number_total             5606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03912g2.cif
_cod_data_source_block           eb113t_g
_cod_depositor_comments
'Adding full bibliography for 7049077--7049089.cif.'
_cod_original_cell_volume        1995.77(15)
_cod_database_code               7049084
_chemical_oxdiff_formula         C18H20N3PtI3
_chemical_oxdiff_usercomment     'Clear, yellow, block 0.2 0.2 0.1'
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.175
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N3-C11 \\sim N3-C11A
 with sigma of 0.02
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 I3-C13 \\sim I3A-C13A
 with sigma of 0.02
 C12-N3 \\sim N3-C12A
 with sigma of 0.02
 I3-C11 \\sim I3A-C11A
 with sigma of 0.02
3. Restrained planarity
 I3A, C11A, C12A, C13A, C14A, C15A, C16A, C17A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C17) = Uanis(C17A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
5. Others
 Sof(I3A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(C13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=1-FVAR(1)
 Sof(I3)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(C13)=Sof(C14)=Sof(H14)=
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C11A(H11C,H11D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C15(H15), C16(H16), C17(H17), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A)
6.c Fitted hexagon refined as free rotating group:
 C12A(C13A,C14A,C15A,C16A,C17A)
;
_shelx_res_checksum              56371
_shelx_shelxl_version_number     2014/7
_ins_header
;
TITL EB113T_g in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 0.71073   8.984819  17.111393  13.364423  90.0000 103.7540  90.0000
ZERR    4.00   0.000407   0.000785   0.000482   0.0000   0.0040   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N I Pt
UNIT 72.00 80.00 12.00 12.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'