Ruthenaphosphaalkenyls: Synthesis, Structures, and Their Conversion to η2-Phosphaalkene Complexes
Greenacre, Victoria K.; Trathen, Nicola; Crossley, Ian R.; Organometallics 34 (2015) 2533–; doi:10.1021/om5012177

data_4085714
_publ_section_title
;
 Ruthenaphosphaalkenyls: Synthesis, Structures, and Their Conversion to
 \h2-Phosphaalkene Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2533
_journal_paper_doi               10.1021/om5012177
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C47 H44 Cl O P3 Ru Si'
_chemical_formula_sum            'C47 H44 Cl O P3 Ru Si'
_chemical_formula_weight         882.34
_chemical_name_systematic
;
 ?
;
_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             2014-11-24
_audit_creation_method
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Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
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_cell_length_b                   12.0013(2)
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_cell_measurement_reflns_used    14538
_cell_measurement_temperature    173
_cell_measurement_theta_max      61.8230
_cell_measurement_theta_min      4.4100
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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;
  1 omega  -18.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2301  -38.0000    0.0000 42

  2 omega  -29.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2301  -38.0000   30.0000 70

  3 omega   29.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2301   57.0000 -180.0000 26

  4 omega  -27.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.2301  -57.0000  -90.0000 79

  5 omega   23.00   56.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -30.0000    0.0000 33

  6 omega   23.00   49.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -61.0000  -60.0000 26

  7 omega   19.00   49.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -30.0000  120.0000 30

  8 omega   18.00   44.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -95.0000  120.0000 26

  9 omega   21.00   47.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000 -125.0000  -30.0000 26

 10 omega   69.00   94.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000 -125.0000  -30.0000 25

 11 omega   19.00   71.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -45.0000  -30.0000 52

 12 omega  106.00  151.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000   45.0000  -60.0000 45

 13 omega   58.00   83.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -95.0000   60.0000 25

 14 omega   55.00   98.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -61.0000  -60.0000 43

 15 omega   78.00  104.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000   45.0000 -150.0000 26

 16 omega   87.00  112.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -77.0000 -120.0000 25

 17 omega   26.00   69.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -77.0000 -120.0000 43

 18 omega   31.00   68.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -45.0000 -120.0000 37

 19 omega   18.00   43.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -30.0000  -90.0000 25

 20 omega   56.00   82.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -95.0000  120.0000 26

 21 omega   26.00   56.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -30.0000  -30.0000 30

 22 omega   26.00   73.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -45.0000   60.0000 47

 23 omega   60.00   87.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000   15.0000  -30.0000 27

 24 omega  106.00  149.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000   15.0000  -30.0000 43

 25 omega   23.00   48.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -45.0000  -60.0000 25

 26 omega   21.00   89.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000 -125.0000  -90.0000 68

 27 omega   69.00   94.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000 -125.0000   60.0000 25

 28 omega   97.00  122.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000   98.0000   13.0000 25

 29 omega   84.00  122.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  125.0000  -30.0000 38

 30 omega   71.00   97.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -77.0000  150.0000 26

 31 omega   59.00   85.00   1.0000   65.0000
omega____ theta____ kappa____ phi______ frames
    -       86.5000  -65.0000 -110.4806 26
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_radiation_type           CuK\a
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_diffrn_reflns_limit_h_max       22
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_diffrn_reflns_limit_k_max       13
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_diffrn_source                   'sealed X-ray tube'
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light orange'
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.8128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5012177_si_003.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 4085712--4085714.cif.'
_cod_original_cell_volume        4176.0(2)
_cod_database_code               4085714
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         RuSiOP3C45H46
_reflns_odcompleteness_completeness 87.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C72(H72), C43(H43), C51(H51), C10(H10), C25(H25), C73(H73), C61(H61),
 C71(H71), C9(H9), C75(H75), C41(H41), C24(H24), C34(H34), C54(H54), C42(H42),
 C7(H7), C21(H21), C6(H6), C33(H33), C35(H35), C31(H31), C74(H74), C44(H44),
 C45(H45), C65(H65), C1(H1), C32(H32), C52(H52), C64(H64), C53(H53), C23(H23),
 C62(H62), C22(H22), C63(H63), C55(H55)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'