Solid‒State Molecular Organometallic Chemistry. Single‒Crystal to Single‒Crystal Reactivity and Catalysis with Light Hydrocarbon Substrates.
Chadwick, Fredrick M.; McKay, Alasdair I.; Martinez-Martinez, Antonio J.; Rees, Nick; Kraemer, Tobias; Macgregor, Stuart Alan; Weller, Andrew; Chem. Sci.  (2017) –; doi:10.1039/C7SC01491K

data_1546506
_publ_section_title
;
 Solid--State Molecular Organometallic Chemistry. Single--Crystal to
 Single--Crystal Reactivity and Catalysis with Light Hydrocarbon
 Substrates.
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01491K
_journal_year                    2017
_chemical_formula_moiety         'C32 H12 B F24, C30 H56 P2 Rh'
_chemical_formula_sum            'C62 H68 B F24 P2 Rh'
_chemical_formula_weight         1444.82
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.310(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1979(10)
_cell_length_b                   17.1549(15)
_cell_length_c                   19.9732(12)
_cell_measurement_reflns_used    6309
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.9850
_cell_measurement_theta_min      4.0590
_cell_volume                     6577.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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   -128.00 -36.00   1.00   10.00    --  -40.77-178.00 120.00   92
  2  \w    -12.00  32.00   1.00   10.00    --  -40.77  37.00 -60.00   44
  3  \w    -48.00  29.00   1.00   10.00    --  -40.77  37.00  90.00   77
  4  \w    -49.00 -21.00   1.00   10.00    --  -40.77  37.00   0.00   28
  5  \w   -123.00 -81.00   1.00   10.00    --  -40.77 178.00 -60.00   42
  6  \w     69.00 158.00   1.00   45.00    --  111.00  15.00 -90.00   89
  7  \w     47.00  77.00   1.00   45.00    --  111.00 -94.00 120.00   30
  8  \w     37.00  75.00   1.00   45.00    --  111.00 -30.00  90.00   38
  9  \w     50.00 121.00   1.00   45.00    --  111.00-125.00 -30.00   71
 10  \w     77.00 104.00   1.00   45.00    --  111.00 -94.00-180.00   27
 11  \w     82.00 108.00   1.00   45.00    --  111.00 -94.00  30.00   26
 12  \w     64.00 137.00   1.00   45.00    --  111.00 -61.00 -60.00   73
 13  \w     44.00  71.00   1.00   45.00    --  111.00 -94.00  30.00   27
 14  \w     83.00 169.00   1.00   45.00    --  111.00  61.00  90.00   86
 15  \w     35.00  60.00   1.00   45.00    --  111.00 -94.00  60.00   25
 16  \w     40.00  85.00   1.00   45.00    --  111.00 -30.00 120.00   45
 17  \w     69.00 100.00   1.00   45.00    --  111.00 -94.00  60.00   31
 18  \w     40.00  90.00   1.00   45.00    --  111.00 -45.00-180.00   50
 19  \w     42.00  90.00   1.00   45.00    --  111.00 -30.00-180.00   48
 20  \w    100.00 125.00   1.00   45.00    --  111.00 125.00 -90.00   25
 21  \w     48.00 109.00   1.00   45.00    --  111.00 -94.00 -30.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18456
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.824
_diffrn_reflns_theta_min         4.097
_exptl_absorpt_coefficient_mu    3.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
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    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6753
_refine_ls_number_restraints     237
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.1019
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+59.6037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2487
_refine_ls_wR_factor_ref         0.2542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5852
_reflns_number_total             6753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01491k3.cif
_cod_data_source_block           1butene
_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 
;
_cod_database_code               1546506
_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
 F7-F8 \\sim F7-F9 \\sim F8-F9 \\sim F7A-F8A \\sim F7A-F9A \\sim F8A-F9A
 with sigma of 0.04
 C32-F7 \\sim C32-F8 \\sim C32-F9 \\sim C32-F7A \\sim C32-F8A \\sim C32-F9A
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F3A-F1A \\sim F3A-F2A \\sim F1A-F2A
 with sigma of 0.04
 C24-F1 \\sim C24-F2 \\sim C24-F3 \\sim C24-F3A \\sim C24-F1A \\sim C24-F2A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim C2 \\sim C3 \\sim C1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C32 \\sim F9 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
F9A \\sim C32 \\sim F7A \\sim F8A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C24 \\sim F1 \\sim F2 \\sim F3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C24 \\sim F3A \\sim F1A \\sim F2A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C4, C2, C3, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, F7, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, F7A, F8A, F9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, F3A, F1A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(1)
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Fixed Sof: C3(0.5) H3(0.5) C2(0.5) H2(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C12(H12A,H12B), C6(H6A,H6B), C8(H8A,H8B), C15(H15A,H15B),
 C10(H10A,H10B), C14(H14A,H14B), C9(H9A,H9B), C7(H7A,H7B), C13(H13A,H13B),
 C17(H17A,H17B)
6.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C19(H19), C27(H27), C31(H31), C23(H23), C21(H21), C3(H3), C2(H2)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              42479
_olex2_date_sample_data_collection 2016-11-19
_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
;