Through-conjugation of two phosphaalkyne ('C[triple bond, length as m-dash]P') moieties mediated by a bimetallic scaffold.
Leech, Matthew C.; Crossley, Ian R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4428–4432; doi:10.1039/c8dt00110c

data_7045754
_publ_section_exptl_refinement
'The two triflate counter ions were disorderd and could not be modelled.  The associated electron density was therefore treat with SQUEEZE.'
_publ_section_title
;
 Through-conjugation of two phosphaalkyne ('C[triple bond, length as
 m-dash]P') moieties mediated by a bimetallic scaffold.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4428
_journal_page_last               4432
_journal_paper_doi               10.1039/c8dt00110c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C122 H118 P10 Ru2 Si2'
_chemical_formula_sum            'C122 H118 P10 Ru2 Si2'
_chemical_formula_weight         2152.18
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-15 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                95.011(2)
_cell_angle_beta                 90.319(2)
_cell_angle_gamma                91.956(2)
_cell_formula_units_Z            2
_cell_length_a                   14.3964(4)
_cell_length_b                   19.4639(5)
_cell_length_c                   23.3880(5)
_cell_measurement_reflns_used    15881
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.3920
_cell_measurement_theta_min      3.6020
_cell_volume                     6524.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00   3.00   1.00    5.00    --    0.00 -57.00  60.00   71
  2  \w    -26.00  70.00   1.00    5.00    --    0.00  77.00-180.00   96
  3  \w   -112.00 -34.00   1.00   25.00    --  -54.75 125.00 120.00   78
  4  \w    -69.00 -32.00   1.00   25.00    --  -54.75 125.00 -60.00   37
  5  \w     29.00 122.00   1.00   25.00    --   54.75  38.00-180.00   93
  6  \w     73.00 102.00   1.00   25.00    --   54.75 125.00  60.00   29
  7  \w     76.00 107.00   1.00   25.00    --   54.75 125.00   0.00   31
  8  \w     73.00 119.00   1.00   25.00    --   54.75 125.00  90.00   46
  9  \w    -18.00  80.00   1.00   25.00    --   54.75 -38.00   0.00   98
 10  \w      1.00  62.00   1.00   25.00    --   54.75 -77.00-120.00   61
 11  \w     36.00 104.00   1.00   65.00    --  109.50 178.00-120.00   68
 12  \w     41.00 124.00   1.00   65.00    --  109.50 -38.00 120.00   83
 13  \w     37.00 100.00   1.00   65.00    --  109.50   0.00 -60.00   63
 14  \w     40.00 135.00   1.00   65.00    --  109.50 -92.00   0.00   95
 15  \w     45.00 131.00   1.00   65.00    --  109.50 -50.00-150.00   86
 16  \w     98.00 172.00   1.00   65.00    --  109.50  64.00  60.00   74
 17  \w     39.00 131.00   1.00   65.00    --  109.50 -50.00   0.00   92
 18  \w     89.00 177.00   1.00   65.00    --  109.50  64.00 150.00   88
 19  \w    122.00 171.00   1.00   65.00    --  109.50   0.00 -60.00   49
 20  \w     46.00 107.00   1.00   65.00    --  109.50 -93.00 158.03   61
 21  \w     52.00 129.00   1.00   65.00    --  109.50 -93.00-130.06   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0134849000
_diffrn_orient_matrix_UB_12      0.0585506000
_diffrn_orient_matrix_UB_13      -0.0397625000
_diffrn_orient_matrix_UB_21      -0.0254504000
_diffrn_orient_matrix_UB_22      0.0531321000
_diffrn_orient_matrix_UB_23      0.0496577000
_diffrn_orient_matrix_UB_31      0.1031303000
_diffrn_orient_matrix_UB_32      0.0083240000
_diffrn_orient_matrix_UB_33      0.0180433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41580
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.625
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.100
_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     1369
_refine_ls_number_reflns         23612
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0611
_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^)+(0.1067P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18345
_reflns_number_total             23612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00110c3.cif
_cod_data_source_block           mcl15-044c
_cod_depositor_comments          'Adding full bibliography for 7045754.cif.'
_cod_original_cell_volume        6524.4(3)
_cod_database_code               7045754
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ru2 P10 Si2 S2 F6 O6 C124 H118'
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.439
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C124, C125, C126, C127, C128, C129
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C130, C135
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C79, C84
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C73, C74, C75, C76, C77, C78
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C110
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99, C100, C101, C102, C103, C104
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C100, C101, C142, C143, C144, C145
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C110, C109, C108, C107, C106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C136, C141, C140, C139, C138, C137
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C130 \\sim C135: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C79 \\sim C84: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C105 \\sim C110: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C100 \\sim C101 \\sim C142 \\sim C143 \\sim C144 \\sim C145: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C105 \\sim C110 \\sim C109 \\sim C108 \\sim C107 \\sim C106: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C136 \\sim C141 \\sim C140 \\sim C139 \\sim C138 \\sim C137: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H72C)=Sof(H72D)=Sof(C123)=Sof(H12A)=Sof(H12B)=Sof(C124)=Sof(C125)=
 Sof(H125)=Sof(C126)=Sof(H126)=Sof(C127)=Sof(H127)=Sof(C128)=Sof(H128)=
 Sof(C129)=Sof(H129)=Sof(C130)=Sof(C135)=Sof(H135)=Sof(C134)=Sof(H134)=
 Sof(C133)=Sof(H133)=Sof(C132)=Sof(H132)=Sof(C131)=Sof(H131)=1-FVAR(1)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(C74)=Sof(H74)=
 Sof(C75)=Sof(H75)=Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C78)=Sof(H78)=
 Sof(C79)=Sof(C84)=Sof(H84)=Sof(C83)=Sof(H83)=Sof(C82)=Sof(H82)=Sof(C81)=
 Sof(H81)=Sof(C80)=Sof(H80)=FVAR(1)
 Sof(C136)=Sof(C137)=Sof(H137)=Sof(C138)=Sof(H138)=Sof(C139)=Sof(H139)=
 Sof(C140)=Sof(H140)=Sof(C141)=Sof(H141)=1-FVAR(2)
 Sof(C105)=Sof(C110)=Sof(H110)=Sof(C109)=Sof(H109)=Sof(C108)=Sof(H108)=
 Sof(C107)=Sof(H107)=Sof(C106)=Sof(H106)=FVAR(2)
 Sof(H10A)=Sof(H10B)=Sof(C142)=Sof(C143)=Sof(H143)=Sof(C144)=Sof(H144)=
 Sof(C145)=Sof(H145)=1-FVAR(3)
 Sof(C99)=Sof(H100)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=
 Sof(C104)=Sof(H104)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C45(H45A,H45B), C46(H46A,H46B), C71(H71A,
 H71B), C72(H72A,H72B), C72(H72C,H72D), C97(H97A,H97B), C98(H98A,H98B),
 C123(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55),
  C56(H56), C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C84(H84), C83(H83), C82(H82), C81(H81),
 C80(H80), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93),
  C94(H94), C95(H95), C96(H96), C100(H100), C100(H10A), C101(H101), C101(H10B),
 C102(H102), C103(H103), C104(H104), C110(H110), C109(H109), C108(H108),
 C107(H107), C106(H106), C112(H112), C113(H113), C114(H114), C115(H115),
 C116(H116), C118(H118), C119(H119), C120(H120), C121(H121), C122(H122),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C135(H135),
 C134(H134), C133(H133), C132(H132), C131(H131), C137(H137), C138(H138),
 C139(H139), C140(H140), C141(H141), C143(H143), C144(H144), C145(H145)
5.c Fitted hexagon refined as free rotating group:
 C73(C74,C75,C76,C77,C78), C79(C84,C83,C82,C81,C80), C99(C100,C101,C102,C103,
 C104), C105(C110,C109,C108,C107,C106), C124(C125,C126,C127,C128,C129),
 C130(C135,C134,C133,C132,C131)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_olex2_date_sample_data_collection 2016-05-31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.409
_oxdiff_exptl_absorpt_empirical_full_min 0.824