Increasing phosphorescent quantum yields and lifetimes of platinum-alkynyl complexes with extended conjugation
Zhang, Yuzhen; Hauke, Cory E.; Crawley, Matthew R.; Schurr, Bradley E.; Fulong, Cressa Ria P.; Cook, Timothy; Dalton Trans.  (2017) –; doi:10.1039/C7DT01817G

data_7043501
_publ_section_title
;
 Increasing phosphorescent quantum yields and lifetimes of
 platinum-alkynyl complexes with extended conjugation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01817G
_journal_year                    2017
_chemical_formula_moiety         'C26 H38 N2 P2 Pt'
_chemical_formula_sum            'C26 H38 N2 P2 Pt'
_chemical_formula_weight         635.61
_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
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-26 deposited with the CCDC.
2017-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0413(4)
_cell_length_b                   10.8299(5)
_cell_length_c                   14.3021(6)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    99.67
_cell_measurement_theta_max      28.349
_cell_measurement_theta_min      3.039
_cell_volume                     1336.57(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14476
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.347
_diffrn_reflns_theta_min         3.528
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.384
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0754 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.7998. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slow evaporation from methanol'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.513
_refine_diff_density_min         -1.971
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+1.0180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2904
_reflns_number_total             3318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01817g3.cif
_cod_data_source_block           4
_cod_database_code               7043501
_shelx_shelxl_version_number     2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C10(H10a,H10b), C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C11(H11a,H11b,H11c)
;
_olex2_exptl_crystal_mounting_method 'MiTeGen MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'