An efficient room-temperature synthesis of highly phosphorescent styrenic Pt(ii) complexes and their polymerization by ATRP
Mayder, Don M.; Thompson, Kyle A.; Christopherson, Cheyenne J.; Paisley, Nathan R.; Hudson, Zachary M.; Polymer Chemistry 9 (2018) 5418–; doi:10.1039/C8PY01337C

data_1550140
_publ_section_title
;
 An efficient room-temperature synthesis of highly phosphorescent styrenic
 Pt(ii) complexes and their polymerization by ATRP
;
_journal_issue                   45
_journal_name_full               'Polymer Chemistry'
_journal_page_first              5418
_journal_paper_doi               10.1039/C8PY01337C
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H21 F2 N O2 Pt'
_chemical_formula_sum            'C25 H21 F2 N O2 Pt'
_chemical_formula_weight         600.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-09-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0937(13)
_cell_length_b                   11.3331(6)
_cell_length_c                   6.7354(3)
_cell_measurement_reflns_used    8147
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.33
_cell_measurement_theta_min      2.34
_cell_volume                     2068.14(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            23144
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.559
_diffrn_reflns_theta_min         1.503
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.825
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0846 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.7409. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and hexane by slow evaporation'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.477
_refine_diff_density_min         -2.987
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details
;
 Flack x determined using 1470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5898
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0125P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                4427
_reflns_number_total             5898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01337c2.cif
_cod_data_source_block           zh014
_cod_depositor_comments
'Adding full bibliography for 1550139--1550142.cif.'
_cod_database_code               1550140
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.291
_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. 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
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24)
3.c X=CH2 refined with riding coordinates:
 C25(H25A,H25B)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              5043
_olex2_date_sample_data_collection 2018-04-05
_olex2_date_sample_submission    2018-03-28
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id DMM-I-30
_olex2_submission_special_instructions 'No special instructions were received'