Carbon(0)-Bridged Pt/Ag Dinuclear and Tetranuclear Complexes Based on a Cyclometalated Pincer Carbodiphosphorane Platform
Kubo, Kazuyuki; Okitsu, Hiroyuki; Miwa, Hiroto; Kume, Shoko; Cavell, Ronald G.; Mizuta, Tsutomu; Organometallics 36 (2017) 266–; doi:10.1021/acs.organomet.6b00700

data_4086973
_publ_section_title
;
 Carbon(0)-Bridged Pt/Ag Dinuclear and Tetranuclear Complexes Based on a
 Cyclometalated Pincer Carbodiphosphorane Platform
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              266
_journal_paper_doi               10.1021/acs.organomet.6b00700
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C43 H43 Ag P3 Pt, C4 H10 O, C F3 O3 S'
_chemical_formula_sum            'C48 H53 Ag F3 O4 P3 Pt S'
_chemical_formula_weight         1178.83
_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
_audit_creation_date             2016-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                112.810(2)
_cell_angle_beta                 106.210(2)
_cell_angle_gamma                102.5800(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5033(14)
_cell_length_b                   14.6582(16)
_cell_length_c                   15.264(3)
_cell_measurement_reflns_used    9213
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.419
_cell_volume                     2302.1(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (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  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13146
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.582
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.665
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0717 before and 0.0196 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.355
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9997
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0320P)^2^+4.2561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9284
_reflns_number_total             9997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00700_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2302.2(5)
_cod_database_code               4086973
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.609
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C48-C47 = C46-C45
 1.49 with sigma of 0.02
 O4-C47 = O4-C45
 1.42 with sigma of 0.01
 C48-O4
 2.38 with sigma of 0.02
 O4-C46
 2.38 with sigma of 0.02
 C47-C45
 2.37 with sigma of 0.02
3. Rigid bond restraints
 C46, C45, O4, C47, C48
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C43A, C43, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C46 \\sim C45 \\sim O4 \\sim C47 \\sim C48: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C43A \\sim C43 \\sim C42: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
5. Others
 Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B), C42(H42C,H42D), C45(H45A,
 H45B), C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C33(H33), C34(H34), C35(H35), C36(H36)
6.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C43A(H43D,H43E,
 H43F), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              74736
_shelx_hkl_checksum              35154
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'