Axial Tri-tert-butylphosphane Coordination to Rh2(OAc)4: Synthesis, Structure, and Catalytic Studies
Tan, Jiantao; Kuang, Yi; Wang, Yi; Huang, Qingfei; Zhu, Jin; Wang, Yuanhua; Organometallics 35 (2016) 3139–; doi:10.1021/acs.organomet.6b00477

data_4086704
_publ_section_title
;
 Axial Tri-tert-butylphosphane Coordination to Rh2(OAc)4: Synthesis,
 Structure, and Catalytic Studies
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3139
_journal_paper_doi               10.1021/acs.organomet.6b00477
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C44 H78 O8 P2 Rh2'
_chemical_formula_sum            'C44 H78 O8 P2 Rh2'
_chemical_formula_weight         1002.82
_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             2016-01-14
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_cell_angle_alpha                68.778(3)
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_cell_formula_units_Z            2
_cell_length_a                   11.3382(3)
_cell_length_b                   14.2991(4)
_cell_length_c                   16.3895(7)
_cell_measurement_reflns_used    11111
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.6690
_cell_measurement_theta_min      4.5930
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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;
  1 omega  -31.00   63.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -77.0000   30.0000 94

  2 omega   18.00  106.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   38.0000  -90.0000 88

  3 omega   20.00  104.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000  120.0000 84

  4 omega   23.00   90.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171 -125.0000 -180.0000 67

  5 omega   18.00  106.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   38.0000    0.0000 88

  6 omega  -33.00   55.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -38.0000  -60.0000 88

  7 omega    1.00   75.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
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  8 omega   10.00  104.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   77.0000   60.0000 94

  9 omega   20.00  104.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000 -180.0000 84

 10 omega    1.00   75.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -99.0000  -90.0000 74

 11 omega   39.00  109.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 70

 12 omega   40.00   98.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

 13 omega   40.00   98.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 58

 14 omega   39.00  109.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 15 omega   38.00  116.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 78

 16 omega   40.00  135.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   30.0000 95

 17 omega   40.00   98.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

 18 omega   38.00   91.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 19 omega   91.00  176.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   90.0000 85

 20 omega   40.00   98.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 58

 21 omega   40.00   98.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 22 omega   38.00   91.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 23 omega  100.00  178.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 78

 24 omega   38.00   91.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 25 omega   39.00  109.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 70

 26 omega   38.00   91.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 27 omega   39.00  177.00   1.0000    6.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -120.0000 138

 28 omega  -35.00   66.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -19.0000  120.0000 101

 29 omega  -33.00   55.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -38.0000   60.0000 88

 30 omega   10.00  104.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   77.0000    0.0000 94

 31 omega   20.00  104.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   57.0000  -60.0000 84

 32 omega    0.00   26.00   1.0000    1.6300
omega____ theta____ kappa____ phi______ frames
    -       36.4171   94.0000 -140.2549 26
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0155874000
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_diffrn_orient_matrix_UB_23      -0.0036423000
_diffrn_orient_matrix_UB_31      0.1238645000
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_diffrn_orient_matrix_UB_33      -0.0306052000
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_number            25730
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        67.079
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_diffrn_reflns_theta_min         4.575
_diffrn_source                   'Enhance (Cu) X-ray Source'
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
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_exptl_crystal_colour_modifier   reddish
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_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1052
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_refine_diff_density_max         1.000
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_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0481
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+0.3631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7578
_reflns_number_total             8694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00477_si_002.cif
_cod_data_source_block           wyh-tjt-0278
_cod_original_cell_volume        2433.09(15)
_cod_database_code               4086704
_reflns_odcompleteness_completeness 99.92
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I), C00J(H00J), C00X(H0AA)
2.b Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00O(H00K,H00L), C00P(H00M,H00N), C00Q(H00O,H00P), C00R(H00Q,
 H00R), C00S(H00S,H00T), C00T(H00U,H00V), C00V(H00Z,H), C00W(H00,HA), C00Y(H1AA,
 HB), C00Z(H2AA,HC), C010(H01A,H01B), C011(H01C,H01D), C012(H01E,H01F),
 C013(H01G,H01H), C014(H01I,H01J), C015(H01K,H01L), C016(H01M,H01N), C017(H01O,
 H01P), C018(H01Q,H01R), C019(H01S,H01T), C01A(H01U,H01V), C01B(H01W,H01X),
 C01C(H01Y,HD), C01F(H3AA,HI), C01G(H4AA,HJ), C01H(H5AA,HK), C01I(H6AA,HL),
 C01J(H7AA,HM), C01K(H8AA,HN)
2.c Idealised Me refined as rotating group:
 C00N(H00C,H00E,H00G), C00U(H00W,H00X,H00Y), C01D(H01Z,HE,HF), C01E(H01,HG,HH)
;
_shelx_res_checksum              57007
_shelx_hkl_checksum              78863
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-01-13
_olex2_submission_special_instructions 'No special instructions were received'