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_7049078
_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         'C34 H28 I2 N6 Pt, 2(C F3 O3 S)'
_chemical_formula_sum            'C36 H28 F6 I2 N6 O6 Pt S2'
_chemical_formula_weight         1267.65
_chemical_name_systematic
'Bis(2-iodobenzyldi(2-pyridyl)amine)platinum(II) triflate'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-16
_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                 120.9270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0099(4)
_cell_length_b                   11.6891(2)
_cell_length_c                   18.0292(3)
_cell_measurement_reflns_used    5253
_cell_measurement_temperature    170
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      1.00
_cell_volume                     3978.99(13)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2008)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_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      170
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27241
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.756
_diffrn_reflns_theta_min         2.634
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    5.265
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0963 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.8021.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0346
_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^)+32.5326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4413
_reflns_number_total             5155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03912g2.cif
_cod_data_source_block           eb121_meoh_s
_cod_depositor_comments
'Adding full bibliography for 7049077--7049089.cif.'
_cod_original_cell_volume        3978.99(12)
_cod_database_code               7049078
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.588
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C11, C11A}
3. Rigid bond restraints
 C12A, C13A, C14A, C15A, C16A, C17A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma
of 0.008 and sigma for terminal atoms of 0.05
Uanis(C11) = Uanis(C11A)
5. Others
 Sof(I1A)=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(I1)=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              75796
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'