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_4086703
_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         'C16 H33 O4 P Rh'
_chemical_formula_sum            'C16 H33 O4 P Rh'
_chemical_formula_weight         423.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.539(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8038(3)
_cell_length_b                   19.4899(6)
_cell_length_c                   12.0669(4)
_cell_measurement_reflns_used    5176
_cell_measurement_temperature    294.39(10)
_cell_measurement_theta_max      72.4640
_cell_measurement_theta_min      4.3790
_cell_volume                     2021.12(12)
_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
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.39(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega    1.00   75.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   30.0000 74

  2 omega  -31.00   63.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  -90.0000 94

  3 omega   20.00  104.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  120.0000 84

  4 omega  -31.00   53.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  120.0000 84

  5 omega   23.00   90.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -120.0000 67

  6 omega  -33.00   55.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -180.0000 88

  7 omega  100.00  178.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 78

  8 omega   38.00   91.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

  9 omega   40.00   98.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 58

 10 omega   39.00  109.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

 11 omega   38.00   91.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 12 omega   38.00   91.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 13 omega   38.00  116.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 78

 14 omega   40.00   98.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

 15 omega   39.00  109.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 70

 16 omega   70.00  178.00   1.0000   10.5100
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 108

 17 omega   20.00   73.00   1.0000    2.6300
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -90.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0224529000
_diffrn_orient_matrix_UB_12      0.0678387000
_diffrn_orient_matrix_UB_13      -0.0670613000
_diffrn_orient_matrix_UB_21      -0.0144354000
_diffrn_orient_matrix_UB_22      -0.0402001000
_diffrn_orient_matrix_UB_23      -0.1117080000
_diffrn_orient_matrix_UB_31      -0.1773144000
_diffrn_orient_matrix_UB_32      -0.0053375000
_diffrn_orient_matrix_UB_33      -0.0111160000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.062
_diffrn_reflns_theta_max         67.062
_diffrn_reflns_theta_min         4.386
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46062
_exptl_absorpt_correction_type   multi-scan
_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            'dull reddish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description
;
;
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1320P)^2^+4.0110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3286
_reflns_number_total             3621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00477_si_002.cif
_cod_data_source_block           wyh-tjt-0240
_cod_original_cell_volume        2021.12(11)
_cod_database_code               4086703
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H00Y-HE
 2.45 with sigma of 0.01
 H00G-H00U
 2.45 with sigma of 0.01
 H00J-HC
 2.45 with sigma of 0.01
 H00M-H00X
 2.45 with sigma of 0.01
 H-H00T
 2.45 with sigma of 0.01
 H00L-H00P
 2.45 with sigma of 0.01
 H00M-H00V
 2.45 with sigma of 0.01
 H00I-H00U
 2.45 with sigma of 0.01
 H00H-H00W
 2.45 with sigma of 0.01
 H00O-H00V
 2.45 with sigma of 0.01
 HA-H00
 2.45 with sigma of 0.01
 HA-HE
 2.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C007 \\sim C008 \\sim C009 \\sim C00A \\sim C00B \\sim C00C \\sim C00D \\sim
C00E \\sim C00F \\sim C00G \\sim C00H \\sim C00I \\sim C00J \\sim C00K \\sim
C00L \\sim C00M: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
4.a Idealised Me refined as rotating group:
 C00A(H00A,H00B,H00C), C00D(H00D,H00E,H00F), C00E(H00G,H00H,H00I), C00F(H00J,
 H00K,H00L), C00G(H00M,H00N,H00O), C00H(H00P,H00Q,H00R), C00I(H00S,H00T,H00U),
 C00J(H00V,H00W,H00X), C00K(H00Y,H,HA), C00L(H00Z,HB,HC), C00M(H00,HD,HE)
;
_shelx_res_checksum              30230
_shelx_hkl_checksum              73299
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-30
_olex2_submission_special_instructions 'No special instructions were received'