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_4086975
_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 O3 P4 Pt, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C63 H60 Ag Cl2 F3 O6 P4 Pt S'
_chemical_formula_weight         1499.91
_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                89.4128(8)
_cell_angle_beta                 78.9409(8)
_cell_angle_gamma                81.5996(8)
_cell_formula_units_Z            4
_cell_length_a                   13.6883(8)
_cell_length_b                   17.7602(11)
_cell_length_c                   25.7558(15)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.695
_cell_measurement_theta_min      2.319
_cell_volume                     6078.2(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 0.979
_diffrn_measured_fraction_theta_max 0.958
_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  0.0178
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35058
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.968
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.909
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0269 after correction.
The Ratio of minimum to maximum transmission is 0.9136.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1571
_refine_ls_number_reflns         26740
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+9.8637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21742
_reflns_number_total             26740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00700_si_002.cif
_cod_data_source_block           5
_cod_database_code               4086975
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.822
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Cl1-C63 = Cl2A-C63A = Cl2-C63 = Cl1A-C63A
 1.77 with sigma of 0.02
 Cl2C-C63B = Cl2B-C63B = Cl1C-C63B = Cl1B-C63B
 1.77 with sigma of 0.02
 S1C-O5C = S1C-O4C = S1C-O6C = S1B-O6B = S1B-O4B = S1B-O5B
 1.431 with sigma of 0.02
 F1B-C62B = F3B-C62B = F2B-C62B = F1C-C62C = F2C-C62C = F3C-C62C
 1.326 with sigma of 0.02
 F1C-F3C
 2.13 with sigma of 0.04
 F1C-F2C
 2.13 with sigma of 0.04
 F2C-F3C
 2.13 with sigma of 0.04
 F1B-F2B
 2.13 with sigma of 0.04
 F1B-F3B
 2.13 with sigma of 0.04
 F3B-F2B
 2.13 with sigma of 0.04
 O5C-O4C
 2.416 with sigma of 0.04
 O5C-O6C
 2.416 with sigma of 0.04
 O6C-O4C
 2.416 with sigma of 0.04
 O4B-O5B
 2.416 with sigma of 0.04
 O5B-O6B
 2.416 with sigma of 0.04
 O6B-O4B
 2.416 with sigma of 0.04
3. Rigid bond restraints
 Cl2A, C63, Cl1, Cl2, C63A, Cl1A, Cl2C, Cl2B, C63B, Cl1C, Cl1B, C58A, C58, C59,
  C56A, C57, C56, C60A, C60, C61, C60B, C61B, C58B, C58C, C59B, C56C, C56B, C57B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61C, C60C
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Cl2C \\sim Cl2B \\sim C63B \\sim Cl1C \\sim Cl1B \\sim Cl1 \\sim C63 \\sim Cl2A
\\sim Cl2 \\sim C63A \\sim Cl1A \\sim C59 \\sim C58 \\sim C58A \\sim C56A \\sim
C57 \\sim C56 \\sim C60 \\sim C60A \\sim C61 \\sim C61B \\sim C60B \\sim C58C
\\sim C58B \\sim C59B \\sim C56B \\sim C56C \\sim C57B: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C61C \\sim C60C: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.02
Uanis(C60C) \\sim Ueq, Uanis(C61C) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
5. Others
 Sof(Cl2A)=Sof(Cl1A)=Sof(C63A)=Sof(H63G)=Sof(H63H)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C63)=Sof(H63E)=Sof(H63F)=FVAR(1)
 Sof(H63C)=Sof(H63D)=Sof(Cl1C)=Sof(Cl2C)=1-FVAR(2)
 Sof(Cl1B)=Sof(Cl2B)=Sof(H63A)=Sof(H63B)=FVAR(2)
 Sof(H57J)=Sof(H57K)=Sof(H57L)=Sof(H61J)=Sof(H61K)=Sof(H61L)=Sof(H59J)=
 Sof(H59K)=Sof(H59L)=Sof(C58A)=Sof(H58G)=Sof(H58H)=Sof(C60A)=Sof(H60G)=
 Sof(H60H)=Sof(C56A)=Sof(H56G)=Sof(H56H)=1-FVAR(3)
 Sof(H57G)=Sof(H57H)=Sof(H57I)=Sof(C56)=Sof(H56E)=Sof(H56F)=Sof(H61G)=
 Sof(H61H)=Sof(H61I)=Sof(C58)=Sof(H58E)=Sof(H58F)=Sof(H59G)=Sof(H59H)=Sof(H59I)=
 Sof(C60)=Sof(H60E)=Sof(H60F)=FVAR(3)
 Sof(H57D)=Sof(H57E)=Sof(H57F)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C61C)=
 Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C60C)=Sof(H60C)=Sof(H60D)=Sof(C56C)=
 Sof(H56C)=Sof(H56D)=Sof(C58C)=Sof(H58C)=Sof(H58D)=1-FVAR(4)
 Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C56B)=Sof(H56A)=Sof(H56B)=Sof(H59A)=
 Sof(H59B)=Sof(H59C)=Sof(C60B)=Sof(H60A)=Sof(H60B)=Sof(C61B)=Sof(H61A)=
 Sof(H61B)=Sof(H61C)=Sof(C58B)=Sof(H58A)=Sof(H58B)=FVAR(4)
 Sof(O6C)=Sof(S1C)=Sof(F3C)=Sof(C62C)=Sof(O4C)=Sof(F2C)=Sof(O5C)=Sof(F1C)=1-
 FVAR(5)
 Sof(S1B)=Sof(F2B)=Sof(O4B)=Sof(F3B)=Sof(F1B)=Sof(O5B)=Sof(C62B)=Sof(O6B)=
 FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C56(H56E,H56F), C58(H58E,H58F), C60(H60E,H60F), C63B(H63A,H63B), C63B(H63C,
 H63D), C63(H63E,H63F), C56B(H56A,H56B), C60B(H60A,H60B), C58B(H58A,H58B),
 C58A(H58G,H58H), C60A(H60G,H60H), C56A(H56G,H56H), C60C(H60C,H60D), C56C(H56C,
 H56D), C58C(H58C,H58D), C63A(H63G,H63H)
6.b Aromatic/amide H refined with riding coordinates:
 C27B(H27B), C36B(H36B), C33B(H33B), C21(H21), C36(H36), C18B(H18B), C10(H10),
 C9(H9), C13B(H13B), C35B(H35B), C24(H24), C25B(H25B), C13(H13), C17(H17),
 C18(H18), C27(H27), C21B(H21B), C31(H31), C34B(H34B), C25(H25), C33(H33),
 C35(H35), C10B(H10B), C11(H11), C16(H16), C9B(H9B), C23(H23), C49(H49),
 C34(H34), C15(H15), C47(H47), C22(H22), C30(H30), C15B(H15B), C12(H12),
 C55B(H55B), C17B(H17B), C48(H48), C24B(H24B), C45(H45), C11B(H11B), C43(H43),
 C12B(H12B), C22B(H22B), C55(H55), C39(H39), C28(H28), C46(H46), C7(H7), C6(H6),
  C3(H3), C28B(H28B), C31B(H31B), C45B(H45B), C42B(H42B), C16B(H16B), C7B(H7B),
 C39B(H39B), C43B(H43B), C6B(H6B), C30B(H30B), C53(H53), C3B(H3B), C29B(H29B),
 C51(H51), C41B(H41B), C54(H54), C51B(H51B), C23B(H23B), C29(H29), C52(H52),
 C54B(H54B), C40B(H40B), C47B(H47B), C4(H4), C5(H5), C46B(H46B), C49B(H49B),
 C48B(H48B), C4B(H4B), C5B(H5B), C40(H40), C52B(H52B), C41(H41), C42(H42),
 C53B(H53B)
6.c Idealised Me refined as rotating group:
 C57(H57G,H57H,H57I), C57(H57J,H57K,H57L), C61(H61G,H61H,H61I), C61(H61J,H61K,
 H61L), C59(H59G,H59H,H59I), C59(H59J,H59K,H59L), C57B(H57A,H57B,H57C),
 C57B(H57D,H57E,H57F), C59B(H59A,H59B,H59C), C59B(H59D,H59E,H59F), C61B(H61A,
 H61B,H61C), C61C(H61D,H61E,H61F)
;
_shelx_res_checksum              6423
_shelx_hkl_checksum              58088
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'