A convenient method for the generation of {Rh(PNP)}<sup>+</sup> and {Rh(PONOP)}<sup>+</sup> fragments: reversible formation of vinylidene derivatives.
Gyton, Matthew R.; Hood, Thomas M.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2877–2880; doi:10.1039/c8dt05049j

data_7048905
_publ_section_title
;
 A convenient method for the generation of {Rh(PNP)}<sup>+</sup> and
 {Rh(PONOP)}<sup>+</sup> fragments: reversible formation of vinylidene
 derivatives.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2877
_journal_page_last               2880
_journal_paper_doi               10.1039/c8dt05049j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C37 H61 N O2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C69 H73 B F24 N O2 P2 Rh'
_chemical_formula_weight         1579.94
_chemical_melting_point          ?
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2019-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                66.1490(11)
_cell_angle_beta                 73.5696(9)
_cell_angle_gamma                80.0085(9)
_cell_formula_units_Z            2
_cell_length_a                   12.52895(11)
_cell_length_b                   16.71426(19)
_cell_length_c                   20.3652(2)
_cell_measurement_reflns_used    39347
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3320
_cell_measurement_theta_min      3.6470
_cell_volume                     3732.72(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_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      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -70.00  31.00   1.00    1.22    --  -41.82  57.00  30.00  101
  2  \w   -114.00 -14.00   1.00    1.22    --  -41.82 -57.00-120.00  100
  3  \w    -66.00  33.00   1.00    1.22    --  -41.82  37.00-180.00   99
  4  \w      1.00  83.00   1.00    1.22    --   41.82 -99.00-180.00   82
  5  \w     57.00 131.00   1.00    1.22    --   41.82 178.00-120.00   74
  6  \w     94.00 178.00   1.00    4.89    --  107.00 125.00 -30.00   84
  7  \w     35.00 136.00   1.00    4.89    --  107.00 -61.00  90.00  101
  8  \w     81.00 178.00   1.00    4.89    --  107.00  45.00 -30.00   97
  9  \w     24.00 110.00   1.00    4.89    --  107.00 -94.00 -30.00   86
 10  \w     35.00 136.00   1.00    4.89    --  107.00 -61.00 -90.00  101
 11  \w     81.00 178.00   1.00    4.89    --  107.00  45.00 -90.00   97
 12  \w     81.00 178.00   1.00    4.89    --  107.00  45.00-150.00   97
 13  \w     81.00 178.00   1.00    4.89    --  107.00  45.00 120.00   97
 14  \w     34.00 118.00   1.00    4.89    --  107.00-125.00 -90.00   84
 15  \w     34.00 118.00   1.00    4.89    --  107.00-125.00  90.00   84
 16  \w     34.00 118.00   1.00    4.89    --  107.00-125.00-180.00   84
 17  \w     78.00 178.00   1.00    4.89    --  107.00  61.00   0.00  100
 18  \w     35.00 136.00   1.00    4.89    --  107.00 -61.00  30.00  101
 19  \w     81.00 178.00   1.00    4.89    --  107.00  45.00 -60.00   97
 20  \w     81.00 178.00   1.00    4.89    --  107.00  45.00   0.00   97
 21  \w     24.00 110.00   1.00    4.89    --  107.00 -94.00 150.00   86
 22  \w     34.00 118.00   1.00    4.89    --  107.00-125.00-150.00   84
 23  \w     81.00 178.00   1.00    4.89    --  107.00  45.00  60.00   97
 24  \w     34.00 118.00   1.00    4.89    --  107.00-125.00 -30.00   84
 25  \w     24.00 110.00   1.00    4.89    --  107.00 -94.00 -90.00   86
 26  \w     34.00 118.00   1.00    4.89    --  107.00-125.00  30.00   84
 27  \w     94.00 178.00   1.00    4.89    --  107.00 125.00  30.00   84
 28  \w     35.00 123.00   1.00    4.89    --  107.00-132.00 137.96   88
 29  \w   -114.00 -14.00   1.00    1.22    --  -41.82 -57.00 -30.00  100
 30  \w   -118.00  -9.00   1.00    1.22    --  -41.82 -77.00  90.00  109
 31  \w    -66.00  33.00   1.00    1.22    --  -41.82  37.00 -60.00   99
 32  \w   -118.00  -9.00   1.00    1.22    --  -41.82 -77.00   0.00  109
 33  \w   -118.00  -9.00   1.00    1.22    --  -41.82 -77.00-150.00  109
 34  \w   -114.00 -14.00   1.00    1.22    --  -41.82 -57.00 150.00  100
 35  \w     78.00 125.00   1.00    4.89    --  107.00  61.00 150.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0498219000
_diffrn_orient_matrix_UB_12      -0.0211272000
_diffrn_orient_matrix_UB_13      -0.0699915000
_diffrn_orient_matrix_UB_21      -0.0567506000
_diffrn_orient_matrix_UB_22      -0.0874040000
_diffrn_orient_matrix_UB_23      0.0383218000
_diffrn_orient_matrix_UB_31      -0.1039526000
_diffrn_orient_matrix_UB_32      0.0460055000
_diffrn_orient_matrix_UB_33      -0.0296233000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            72713
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.075
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         6.560
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.166
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.26a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1612
_exptl_crystal_recrystallization_method
'Crystals grown from 1,2-C6H4F2-hexane at 293 K'
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         14165
_refine_ls_number_restraints     1411
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0834P)^2^+5.6404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13328
_reflns_number_total             14165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05049j3.cif
_cod_data_source_block           0452abc18s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048901--7048908.cif.
;
_cod_original_cell_volume        3732.74(8)
_cod_database_code               7048905
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C8-C12 \\sim C8A-C12A \\sim C16A-C10A \\sim C16-C10
 with sigma of 0.01
 C19A-C16A \\sim C18A-C16A \\sim C17A-C16A \\sim C19-C16 \\sim C17-C16 \\sim
C18-C16 \\sim C15A-C12A ~
 C14A-C12A \\sim C13A-C12A \\sim C14-C12 \\sim C15-C12 \\sim C13-C12
 with sigma of 0.01
 C19A-C10A \\sim C18A-C10A \\sim C17A-C10A \\sim C19-C10 \\sim C17-C10 \\sim
C18-C10 \\sim C15A-C8A ~
 C14A-C8A \\sim C13A-C8A \\sim C14-C8 \\sim C15-C8 \\sim C13-C8
 with sigma of 0.01
 C13-C14 \\sim C14-C15 \\sim C15-C13 \\sim C17-C18 \\sim C18-C19 \\sim C19-C17
\\sim C13A-C14A \\sim C14A-
 C15A \\sim C15A-C13A \\sim C17A-C18A \\sim C18A-C19A \\sim C19A-C17A
 with sigma of 0.01
 C7-C12 \\sim C12-C9 \\sim C9-C16 \\sim C16-C11 \\sim C7A-C12A \\sim C12A-C9A
\\sim C9A-C16A \\sim C16A-C11A
 with sigma of 0.01
 C6-C5 \\sim C6A-C5A
 with sigma of 0.01
 C5A-C7A \\sim C5A-C11A
 with sigma of 0.01
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
3. Restrained planarity
 C6, C7, C8, C9, C10, C11, C12, C16
 with sigma of 0.01
 C6A, C7A, C8A, C9A, C10A, C11A, C12A, C16A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4 \\sim C4A \\sim C5 \\sim C5A \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10
\\sim C11 \\sim C16 \\sim C12 \\sim C18 \\sim C17 \\sim C15 \\sim C13 \\sim C14
\\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C16A \\sim
C17A \\sim C19A \\sim C12A \\sim C14A \\sim C13A \\sim C15A \\sim C19 \\sim
C18A \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6
\\sim F6A \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13
\\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F19A \\sim
F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22 \\sim F22A \\sim F23 \\sim F23A
\\sim F24 \\sim F24A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C4) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq,
Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C16A) \\sim Ueq,
Uanis(C17A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20)
\\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A)
\\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C4) = Uanis(C4A) = Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C16) = Uanis(C16A)
5. Others
 Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15D)=
 Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(C9)=Sof(H9)=
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(2)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
6.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,
 H14E,H14F), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C17(H17A,H17B,H17C),
 C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C19(H19A,H19B,
 H19C), C19A(H19D,H19E,H19F)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5A(H5A), C7(H7), C9(H9), C11(H11), C7A(H7A), C9A(H9A), C11A(H11A),
 C22(H22), C23(H23), C24(H24), C202(H202), C204(H204), C206(H206), C210(H210),
 C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226),
 C228(H228), C230(H230)
6.c Fitted hexagon refined as free rotating group:
 C6(C7,C8,C9,C10,C11), C6A(C7A,C8A,C9A,C10A,C11A)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              82151
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.696
_oxdiff_exptl_absorpt_empirical_full_min 0.797