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_4086974
_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         'C61 H58 Ag P4 Pt, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C63 H60 Ag Cl2 F3 O3 P4 Pt S'
_chemical_formula_weight         1451.91
_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
_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                90
_cell_angle_beta                 95.011(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.079(2)
_cell_length_b                   14.147(3)
_cell_length_c                   38.938(7)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.622
_cell_measurement_theta_min      2.201
_cell_volume                     6080(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0218
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            33821
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.901
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0319 after correction.
The Ratio of minimum to maximum transmission is 0.8005.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         13837
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+16.5242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12660
_reflns_number_total             13837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00700_si_002.cif
_cod_data_source_block           4
_cod_original_cell_volume        6080.0(19)
_cod_database_code               4086974
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.670
_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. Rigid bond restraints
 Cl1, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, C65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C64, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, C45A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C44 \\sim C45A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C44 \\sim C45: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl2 \\sim C65: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl1 \\sim C65: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F1 \\sim C64: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F3 \\sim C64: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C64 \\sim F2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
S1 \\sim O2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1 \\sim O3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1 \\sim O1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C42(H42A,H42B), C44(H44A,H44B), C44(H44C,H44D), C65(H65A,H65B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C53(H53), C25(H25), C36(H36), C7(H7), C17(H17), C35(H35), C9(H9),
 C18(H18), C16(H16), C27(H27), C31(H31), C3(H3), C21(H21), C30(H30), C33(H33),
 C29(H29), C13(H13), C34(H34), C4(H4), C51(H51), C12(H12), C22(H22), C10(H10),
 C11(H11), C28(H28), C24(H24), C57(H57), C47(H47), C5(H5), C54(H54), C6(H6),
 C55(H55), C56(H56), C49(H49), C50(H50), C23(H23), C63(H63), C59(H59), C61(H61),
  C48(H48), C60(H60), C62(H62)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C45A(H45D,H45E,
 H45F)
;
_shelx_res_checksum              71804
_shelx_hkl_checksum              47650
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'