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_7048906
_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         'C23 H45 N O P2 Rh, C32 H12 B F24, H2 O'
_chemical_formula_sum            'C55 H59 B F24 N O2 P2 Rh'
_chemical_formula_weight         1397.69
_chemical_melting_point          ?
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-12-10
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.31003(11)
_cell_length_b                   13.31003(11)
_cell_length_c                   35.1489(5)
_cell_measurement_reflns_used    32590
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5260
_cell_measurement_theta_min      3.1060
_cell_volume                     6226.87(11)
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_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    -97.00   1.00   1.00    9.07    --  -23.00 -37.00  30.00   98
  2  \w    -52.00  57.00   1.00    9.07    --   24.41 -77.00 -30.00  109
  3  \w     -4.00  98.00   1.00    9.07    --   24.41  57.00-120.00  102
  4  \w     35.00  83.00   1.00    9.07    --   24.41 178.00 -30.00   48
  5  \w    -50.00  49.00   1.00    9.07    --   24.41 -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      -0.0224764000
_diffrn_orient_matrix_UB_12      0.0100109000
_diffrn_orient_matrix_UB_13      -0.0179013000
_diffrn_orient_matrix_UB_21      0.0387428000
_diffrn_orient_matrix_UB_22      0.0349019000
_diffrn_orient_matrix_UB_23      -0.0041789000
_diffrn_orient_matrix_UB_31      0.0288949000
_diffrn_orient_matrix_UB_32      -0.0389872000
_diffrn_orient_matrix_UB_33      -0.0083283000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            78409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.574
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         3.061
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.26a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_recrystallization_method
'Crystals grown from 1,2-C6H4F2-pentane at 293 K'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 3170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8740
_refine_ls_number_restraints     832
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0662P)^2^+6.5370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8066
_reflns_number_total             8740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05049j3.cif
_cod_data_source_block           0454abc18s
_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        6226.86(13)
_cod_database_code               7048906
_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, All O(H,H) groups
2. Restrained distances
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C307-F1A \\sim C307-F2A \\sim
C307-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
 C203-C207 \\sim C203-C307
 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
 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
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C308-F4A \\sim C308-F5A \\sim
C308-F6A
 with sigma of 0.01
 C205-C208 \\sim C205-C308
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C316-F10A \\sim C316-F11A \\sim
C316-F12A
 with sigma of 0.01
 C213-C216 \\sim C213-C316
 with sigma of 0.01
 F7A-F8A \\sim F8A-F9A \\sim F9A-F7A \\sim F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.01
 C211-F7A \\sim C211-F8A \\sim C211-F9A \\sim C211-F7 \\sim C211-F8 \\sim
C211-F9
 with sigma of 0.01
 C215-F7A \\sim C215-F8A \\sim C215-F9A \\sim C315-F7 \\sim C315-F8 \\sim
C315-F9
 with sigma of 0.01
 C211-C215 \\sim C211-C315
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F10 \\sim F8A \\sim F1 \\sim F7A \\sim F1A \\sim F9A \\sim F2 \\sim F6 \\sim
F2A \\sim F7 \\sim F3 \\sim F8 \\sim F3A \\sim F9 \\sim F4 \\sim F12 \\sim F5
\\sim F11 \\sim F4A \\sim F5A \\sim F6A \\sim F11A \\sim F10A \\sim F12A \\sim
C307 \\sim C207 \\sim C208 \\sim C308 \\sim C216 \\sim C316 \\sim C215 \\sim
C315: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F10) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F7A)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F6) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F4)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F11A)
\\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(C307) \\sim Ueq,
Uanis(C207) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C308) \\sim Ueq,
Uanis(C216) \\sim Ueq, Uanis(C316) \\sim Ueq, Uanis(C215) \\sim Ueq,
Uanis(C315) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C307) = Uanis(C207)
Uanis(C308) = Uanis(C208)
Uanis(C316) = Uanis(C216)
Uanis(C215) = Uanis(C315)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C307)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C207)=FVAR(1)
 Sof(F8A)=Sof(F7A)=Sof(F9A)=Sof(C315)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C215)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C308)=1-FVAR(3)
 Sof(F6)=Sof(F4)=Sof(F5)=Sof(C208)=FVAR(3)
 Sof(F11A)=Sof(F10A)=Sof(F12A)=Sof(C316)=1-FVAR(4)
 Sof(F10)=Sof(F12)=Sof(F11)=Sof(C216)=FVAR(4)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5) O5(0.5) H5A(0.5) H5B(0.5)
5.a Free rotating group:
 O5(H5A,H5B)
5.b Rotating group:
 O4(H4A,H4B)
5.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B)
5.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C212(H212), C210(H210), C202(H202), C204(H204),
 C214(H214), C206(H206)
5.e 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)
;
_shelx_res_checksum              88425
_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 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.833