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_1550142
_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_formula_moiety         'C26 H25 N O3 Pt'
_chemical_formula_sum            'C26 H25 N O3 Pt'
_chemical_formula_weight         594.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.1943(5)
_cell_length_b                   14.6170(5)
_cell_length_c                   23.1255(9)
_cell_measurement_reflns_used    9480
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.29
_cell_volume                     4455.9(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX DUO'
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            60930
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.588
_diffrn_reflns_theta_min         1.545
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.325
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction. wR2(int) was 0.1161 before and 0.0462 after correction. The ratio of minimum to maximum transmission is 0.6927. The \l/2 correction factor is not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and heptane by slow evaporation'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.159
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         13400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+4.9452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11030
_reflns_number_total             13400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01337c2.cif
_cod_data_source_block           zh021
_cod_depositor_comments
'Adding full bibliography for 1550139--1550142.cif.'
_cod_database_code               1550142
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.703
_shelx_estimated_absorpt_t_min   0.261
_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:
 C17(H17A,H17B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C19(H19),
 C20(H20), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
  C33(H33), C35(H35), C36(H36), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50)
2.c X=CH2 refined with riding coordinates:
 C25(H25A,H25B), C51(H51A,H51B)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C38(H38A,H38B,
 H38C), C42(H42A,H42B,H42C), C52(H52A,H52B,H52C)
;
_shelx_res_checksum              94707
_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-78
_olex2_submission_special_instructions 'No special instructions were received'