Platinum(ii) photo-catalysis for highly selective difluoroalkylation reactions
Zhong, Jian-Ji; Yang, Chen; Chang, Xiao-Yong; Zou, Chao; Lu, Wei; Che, Chi-Ming; Chem. Commun.  (2017) –; doi:10.1039/C7CC03823B

data_7120378
_publ_section_title
;
 Platinum(ii) photo-catalysis for highly selective difluoroalkylation
 reactions
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03823B
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C67 H49 N2 O P2 Pt, B F4, 0.5(C H4 O)'
_chemical_formula_sum            'C67.5 H51 B F4 N2 O1.5 P2 Pt'
_chemical_formula_weight         1257.94
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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     heavy
_audit_creation_date             2016-08-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-14 deposited with the CCDC.
2017-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                97.7440(10)
_cell_angle_beta                 98.3340(10)
_cell_angle_gamma                101.0580(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2381(7)
_cell_length_b                   14.8266(9)
_cell_length_c                   16.8813(10)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.74
_cell_measurement_theta_min      3.08
_cell_volume                     2692.9(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51084
_diffrn_reflns_point_group_measured_fraction_full 0.582
_diffrn_reflns_point_group_measured_fraction_max 0.582
_diffrn_reflns_theta_full        66.804
_diffrn_reflns_theta_max         66.804
_diffrn_reflns_theta_min         2.683
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.949
_exptl_absorpt_correction_T_max  0.4661
_exptl_absorpt_correction_T_min  0.3319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0746 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.7121.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1262
_exptl_crystal_preparation       'recrystallized from solvent'
_exptl_crystal_recrystallization_method MeOH/Hexane
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         11133
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0414P)^2^+1.2219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.221
_reflns_Friedel_fraction_full    0.211
_reflns_Friedel_fraction_max     0.211
_reflns_number_gt                11132
_reflns_number_total             11133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_depositor_comments
;

2017-11-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C135 H102 B2 F8 N4 O3 P4 Pt2'
_cod_original_formula_weight         2515.88
_cod_original_formula_moiety         '2(C67 H49 N2 O P2 Pt), 2(B F4), C H4 O'
_cod_original_formula_units_Z            1
_cod_data_source_file            c7cc03823b2.cif
_cod_data_source_block           cxy475_0m
_cod_database_code               7120378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C69(H69), C70(H70), C71(H71), C72(H72), C75(H75), C77(H77), C80(H80),
 C81(H81), C82(H82), C83(H83), C85(H85), C86(H86), C88(H88), C89(H89), C92(H92),
  C93(H93), C94(H94), C95(H95), C96(H96), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C104(H104), C105(H105), C107(H107), C108(H108),
 C109(H109), C110(H110), C115(H115), C116(H116), C117(H117), C118(H118),
 C120(H120), C121(H121), C124(H124), C125(H125), C126(H126), C127(H127),
 C128(H128), C130(H130), C131(H131), C132(H132), C133(H133), C134(H134), C2(H2),
  C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C48(H48), C49(H49),
  C50(H50), C51(H51), C53(H53), C54(H54), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67)
2.b Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C23(H23A,H23B,H23C), C135(H13A,H13B,H13C)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'