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_7048908
_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         'C39 H65 N P2 Rh, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C72 H79 B Cl2 F24 N P2 Rh'
_chemical_formula_weight         1660.92
_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             2018-11-20
_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                107.1454(14)
_cell_angle_beta                 107.1964(14)
_cell_angle_gamma                99.1527(12)
_cell_formula_units_Z            2
_cell_length_a                   12.48767(18)
_cell_length_b                   17.2204(3)
_cell_length_c                   20.1861(3)
_cell_measurement_reflns_used    47281
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.9240
_cell_measurement_theta_min      2.9820
_cell_volume                     3815.67(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -50.00  49.00   1.00   10.81    --   24.25 -37.00 -90.00   99
  2  \w     -8.00 100.00   1.00   10.81    --   24.25  77.00-180.00  108
  3  \w    -52.00  57.00   1.00   10.81    --   24.25 -77.00 -90.00  109
  4  \w     -8.00 100.00   1.00   10.81    --   24.25  77.00 -30.00  108
  5  \w     -8.00 100.00   1.00   10.81    --   24.25  77.00 -90.00  108
  6  \w     -4.00  97.00   1.00   10.81    --   24.25  57.00-180.00  101
  7  \w    -20.00  65.00   1.00   10.81    --   24.25 -99.00  60.00   85
  8  \w    -96.00 -59.00   1.00   10.81    --  -23.31 -57.00   0.00   37
  9  \w   -110.00 -55.00   1.00   10.81    --  -23.31 178.00  90.00   55
 10  \w   -112.00 -57.00   1.00   10.81    --  -23.31-178.00  60.00   55
 11  \w     34.00 111.00   1.00   10.81    --   24.25-178.00-120.00   77
 12  \w     34.00 111.00   1.00   10.81    --   24.25-178.00-180.00   77
 13  \w      0.00  99.00   1.00   10.81    --   24.25  37.00  90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0559386000
_diffrn_orient_matrix_UB_12      0.0289383000
_diffrn_orient_matrix_UB_13      0.0199691000
_diffrn_orient_matrix_UB_21      0.0025176000
_diffrn_orient_matrix_UB_22      -0.0103121000
_diffrn_orient_matrix_UB_23      0.0318533000
_diffrn_orient_matrix_UB_31      0.0260226000
_diffrn_orient_matrix_UB_32      -0.0325587000
_diffrn_orient_matrix_UB_33      -0.0120059000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97196
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.103
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-hexane at 293 K'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         16797
_refine_ls_number_restraints     864
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+3.9152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14711
_reflns_number_total             16797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05049j3.cif
_cod_data_source_block           0445abc18s
_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        3815.66(11)
_cod_database_code               7048908
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C13A-C12 \\sim C15-C12 \\sim C14-C12 \\sim C14A-C12 \\sim C15A-C12 \\sim
C13-C12
 with sigma of 0.01
 C13A-C8 \\sim C15-C8 \\sim C14-C8 \\sim C14A-C8 \\sim C15A-C8 \\sim C13-C8
 with sigma of 0.01
 C13-C14 \\sim C14-C15 \\sim C15-C13 \\sim C13A-C14A \\sim C14A-C15A \\sim
C15A-C13A
 with sigma of 0.01
 Cl1A-C80A \\sim Cl1-C80 \\sim Cl2-C80 \\sim Cl2A-C80A
 with sigma of 0.01
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim
C207-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim
C203-F3A
 with sigma of 0.01
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C215-F7A \\sim C215-F8A \\sim
C215-F9A
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.01
 C211-F7 \\sim C211-F8 \\sim C211-F9 \\sim C211-F7A \\sim C211-F8A \\sim
C211-F9A
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 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. Uiso/Uaniso restraints and constraints
C15A \\sim C13 \\sim C14A \\sim C15 \\sim C13A \\sim C14 \\sim F1 \\sim F1A
\\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim
F7A \\sim F8 \\sim F8A \\sim F9 \\sim F9A \\sim F10 \\sim F10A \\sim F11 \\sim
F11A \\sim F12 \\sim F12A \\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 \\sim Cl1 \\sim Cl2
\\sim C80 \\sim Cl1A \\sim C80A \\sim Cl2A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C15A) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3)
\\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F8) \\sim
Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9A) \\sim Ueq,
Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\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, Uanis(Cl1)
\\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(Cl1A) \\sim Ueq,
Uanis(C80A) \\sim Ueq, Uanis(Cl2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1) = Uanis(Cl1A)
Uanis(C80) = Uanis(C80A)
Uanis(Cl2A) = Uanis(Cl2)
4. Others
 Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C80A)=Sof(H80A)=Sof(H80B)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(C80)=Sof(H80C)=Sof(H80D)=FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(4)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(4)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(5)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(5)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(6)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(6)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(7)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(7)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C80A(H80A,H80B), C80(H80C,H80D)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C11(H11), 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)
5.c Idealised Me refined as rotating group:
 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),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), 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              93526
_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 2.170
_oxdiff_exptl_absorpt_empirical_full_min 0.426