Platinum-based metallomesogens bearing a Pt(4,6-dfppy)(acac) skeleton: synthesis, photophysical properties and polarised phosphorescence application.
Yang, Xuefeng; Wu, Xiugang; Zhou, Di; Yu, Junting; Xie, Guohua; Bruce, Duncan W.; Wang, Yafei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13368–13377; doi:10.1039/c8dt03017k

data_7047389
_publ_section_title
;
 Platinum-based metallomesogens bearing a Pt(4,6-dfppy)(acac) skeleton:
 synthesis, photophysical properties and polarised phosphorescence
 application.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13368
_journal_page_last               13377
_journal_paper_doi               10.1039/c8dt03017k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C74 H83 F6 N O4 Pt'
_chemical_formula_sum            'C74 H83 F6 N O4 Pt'
_chemical_formula_weight         1359.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-05 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                95.086(5)
_cell_angle_beta                 97.666(3)
_cell_angle_gamma                108.351(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4799(15)
_cell_length_b                   11.2272(17)
_cell_length_c                   32.541(5)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.43
_cell_volume                     3226.3(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.1398
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            26261
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         1.275
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.242
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0983 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.6132. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.768
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         12931
_refine_ls_number_restraints     783
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1139P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8294
_reflns_number_total             12931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03017k1.cif
_cod_data_source_block           zz
_cod_depositor_comments          'Adding full bibliography for 7047389.cif.'
_cod_database_code               7047389
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C40
 1.56 with sigma of 0.02
 C36-C39 \\sim C40-C39 \\sim C40-C41 \\sim C42-C41 \\sim C43-C42
 with sigma of 0.02
 C69-C66 \\sim C70-C69 \\sim C70-C71 \\sim C72-C71 \\sim C73-C72
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C33(H33), C36(H36), C63(H63), C66(H66)
5.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C34(H34A,H34B), C35(H35A,H35B),
 C37(H37A,H37B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,
 H50B), C51(H51A,H51B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B),
 C68(H68A,H68B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C25(H25),
 C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C39(H39), C40(H40), C53(H53),
  C54(H54), C58(H58), C59(H59), C61(H61), C62(H62), C69(H69), C70(H70),
 C71(H71), C72(H72)
5.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C73(H73A,H73B,H73C)
;
_olex2_submission_special_instructions 'No special instructions were received'