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_4086972
_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 P3 Pt'
_chemical_formula_sum            'C43 H43 P3 Pt'
_chemical_formula_weight         847.77
_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             2016-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                88.1345(6)
_cell_angle_beta                 81.6658(6)
_cell_angle_gamma                66.1370(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2192(5)
_cell_length_b                   11.0890(6)
_cell_length_c                   19.7174(11)
_cell_measurement_reflns_used    8456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      2.291
_cell_volume                     1823.20(17)
_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 0.975
_diffrn_measured_fraction_theta_max 0.955
_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  0.0105
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10456
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.089
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.010
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0376 before and 0.0157 after correction.
The Ratio of minimum to maximum transmission is 0.9084.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         8002
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0303P)^2^+1.6009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7636
_reflns_number_total             8002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00700_si_002.cif
_cod_data_source_block           2
_cod_database_code               4086972
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.585
_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 bond restraints
 C39, C38, C38A, C39A, C41, C40, C42, C43A, C42A, C43, C40A, C41A, P3, P3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
P3 \\sim C38 \\sim C39 \\sim C39A \\sim C38A \\sim C40 \\sim C41 \\sim C40A
\\sim C41A \\sim C42 \\sim C43 \\sim C43A \\sim C42A \\sim P3A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C38A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(P3A) \\sim Ueq, Uanis(C40A)
\\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C43A) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=
 Sof(C40A)=Sof(H40C)=Sof(H40D)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(P3A)=
 1-FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(P3)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C38A(H38C,H38D), C40(H40A,H40B), C40A(H40C,H40D), C42(H42A,
 H42B), C42A(H42C,H42D)
5.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)
5.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F), C41(H41A,H41B,H41C), C41A(H41D,
 H41E,H41F), C43(H43A,H43B,H43C), C43A(H43D,H43E,H43F)
;
_shelx_res_checksum              93274
_shelx_hkl_checksum              1392
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'