Tolerant to air σ-alkane complexes by surface modification of single crystalline solid-state molecular organometallics using vapour-phase cationic polymerisation: SMOM@polymer.
Bukvic, Alexander J.; Crivoi, Dana Georgiana; Garwood, Hollie G.; McKay, Alasdair I.; Chen, Thomas T. D.; Martínez-Martínez, Antonio J; Weller, Andrew S.; Chemical communications (Cambridge, England) 56 (2020) 4328–4331; doi:10.1039/d0cc01140a

data_7126241
_publ_section_title
;
 Tolerant to air \s-alkane complexes by surface modification of single
 crystalline solid-state molecular organometallics using vapour-phase
 cationic polymerisation: SMOM@polymer.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4328
_journal_page_last               4331
_journal_paper_doi               10.1039/d0cc01140a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C30 H58 O P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C62 H70 B F24 O P2 Rh'
_chemical_formula_weight         1462.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-10
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                91.699(5)
_cell_angle_beta                 95.671(7)
_cell_angle_gamma                98.347(6)
_cell_formula_units_Z            2
_cell_length_a                   12.8770(13)
_cell_length_b                   13.5514(7)
_cell_length_c                   19.2488(13)
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      74.1170
_cell_measurement_theta_min      3.4640
_cell_volume                     3303.8(4)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_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    -48.00  32.00   1.00    7.50    --  -41.40  37.00  30.00   80
  2  \w    -41.00 -12.00   1.00    7.50    --  -41.40 -77.00   0.00   29
  3  \w    -13.00  32.00   1.00    7.50    --  -41.40  37.00-180.00   45
  4  \w     31.00  96.00   1.00    7.50    --   41.40-125.00 -90.00   65
  5  \w    -79.00 -18.00   1.00    7.50    --  -41.40 125.00  60.00   61
  6  \w   -120.00  -4.00   1.00    7.50    --  -41.40 -19.00-150.00  116
  7  \w     64.00 108.00   1.00   30.00    --  111.00 -94.00-150.00   44
  8  \w     94.00 120.00   1.00   30.00    --  111.00-125.00-120.00   26
  9  \w     88.00 121.00   1.00   30.00    --  111.00-125.00 -30.00   33
 10  \w    100.00 141.00   1.00   30.00    --  111.00 -77.00 -30.00   41
 11  \w    102.00 176.00   1.00   30.00    --  111.00  15.00 -60.00   74
 12  \w    141.00 178.00   1.00   30.00    --  111.00  30.00-120.00   37
 13  \w    137.00 177.00   1.00   30.00    --  111.00  77.00-180.00   40
 14  \w    125.00 171.00   1.00   30.00    --  111.00 125.00 -90.00   46
 15  \w    122.00 178.00   1.00   30.00    --  111.00  30.00-150.00   56
 16  \w    107.00 143.00   1.00   30.00    --  111.00  15.00-180.00   36
 17  \w     91.00 120.00   1.00   30.00    --  111.00  30.00-150.00   29
 18  \w     81.00 129.00   1.00   30.00    --  111.00  77.00-180.00   48
 19  \w     68.00  93.00   1.00   30.00    --  111.00  15.00-180.00   25
 20  \w     48.00  90.00   1.00   30.00    --  111.00 -30.00-120.00   42
 21  \w     65.00  99.00   1.00   30.00    --  111.00 -45.00 -90.00   34
 22  \w     69.00  99.00   1.00   30.00    --  111.00 -45.00 -60.00   30
 23  \w     65.00  90.00   1.00   30.00    --  111.00 -30.00 -60.00   25
 24  \w     58.00  98.00   1.00   30.00    --  111.00 -45.00   0.00   40
 25  \w     51.00  78.00   1.00   30.00    --  111.00 -77.00 -30.00   27
 26  \w     50.00  94.00   1.00   30.00    --  111.00 -94.00 -30.00   44
 27  \w     79.00 121.00   1.00   30.00    --  111.00-125.00  60.00   42
 28  \w     91.00 116.00   1.00   30.00    --  111.00-125.00 120.00   25
 29  \w     91.00 121.00   1.00   30.00    --  111.00-125.00 150.00   30
 30  \w     64.00  91.00   1.00   30.00    --  111.00-125.00  90.00   27
 31  \w     64.00 106.00   1.00   30.00    --  111.00 -94.00 120.00   42
 32  \w     54.00  81.00   1.00   30.00    --  111.00-125.00 120.00   27
 33  \w     40.00  79.00   1.00   30.00    --  111.00 -45.00  60.00   39
 34  \w     68.00 114.00   1.00   30.00    --  111.00  15.00  60.00   46
 35  \w    130.00 157.00   1.00   30.00    --  111.00  15.00  60.00   27
 36  \w     42.00  69.00   1.00   30.00    --  111.00 -45.00-150.00   27
 37  \w     41.00 112.00   1.00   30.00    --  111.00 -61.00-180.00   71
 38  \w     44.00  87.00   1.00   30.00    --  111.00-125.00-180.00   43
 39  \w     30.00  83.00   1.00   30.00    --  111.00 -94.00-180.00   53
 40  \w     36.00  89.00   1.00   30.00    --  111.00 -30.00-180.00   53
 41  \w     41.00  68.00   1.00   30.00    --  111.00 -45.00 -60.00   27
 42  \w     34.00 106.00   1.00   30.00    --  111.00 -94.00 -60.00   72
;
_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  0.0943
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.851
_diffrn_reflns_theta_min         3.943
_exptl_absorpt_coefficient_mu    3.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88597
_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            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.588
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         13564
_refine_ls_number_restraints     601
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1457P)^2^+12.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2537
_refine_ls_wR_factor_ref         0.2993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8537
_reflns_number_total             13564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01140a3.cif
_cod_data_source_block           exp_4230
_cod_depositor_comments
'Adding full bibliography for 7126239--7126241.cif.'
_cod_database_code               7126241
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.540
_shelx_estimated_absorpt_t_min   0.419
_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
 F17-F18 \\sim F18-F16 \\sim F16-F17 \\sim F16A-F18A \\sim F18A-F17A \\sim
F17A-F16A
 with sigma of 0.04
 C54-F16 \\sim C54-F18 \\sim C54-F17 \\sim C54-F17A \\sim C54-F18A \\sim
C54-F16A
 with sigma of 0.02
 F14-F13 \\sim F14-F15 \\sim F13-F15 \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
 with sigma of 0.04
 C53-F14 \\sim C53-F13 \\sim C53-F15 \\sim C53-F13A \\sim C53-F14A \\sim
C53-F15A
 with sigma of 0.02
 F6-F5 \\sim F6-F4 \\sim F5-F4 \\sim F6A-F4A \\sim F6A-F5A \\sim F4A-F5A
 with sigma of 0.04
 C37-F6 \\sim C37-F5 \\sim C37-F4 \\sim C37-F6A \\sim C37-F4A \\sim C37-F5A
 with sigma of 0.02
 F11-F10 \\sim F11-F12 \\sim F10-F12 \\sim F11A-F10A \\sim F11A-F12A \\sim
F10A-F12A
 with sigma of 0.04
 C46-F11 \\sim C46-F10 \\sim C46-F12 \\sim C46-F11A \\sim C46-F10A \\sim
C46-F12A
 with sigma of 0.02
 P2-C21 \\sim P2-C21A
 with sigma of 0.02
 C26A-C21A \\sim C22A-C21A \\sim C26-C21 \\sim C22-C21
 with sigma of 0.02
 C26-C25 \\sim C26A-C25A \\sim C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 C24-C23 \\sim C24A-C23A \\sim C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 C21-C23 \\sim C23-C25 \\sim C25-C21 \\sim C21A-C23A \\sim C23A-C25A \\sim
C25A-C21A
 with sigma of 0.02
 C22-C24 \\sim C24-C26 \\sim C26-C22 \\sim C22A-C24A \\sim C24A-C26A \\sim
C26A-C22A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C54 \\sim F17 \\sim F18 \\sim F16: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C54 \\sim F16A \\sim F18A \\sim F17A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C37 \\sim F4A \\sim F6A \\sim F5A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C37 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C46 \\sim F11 \\sim F12 \\sim F10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C46 \\sim F11A \\sim F12A \\sim F10A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
P2 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P2 \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F16) \\sim Ueq, Uanis(F16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C53, F13, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, F15A, F13A, F14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, F17, F18, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, F16A, F18A, F17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, F5, F6, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C46, F11, F10, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, C21A, C22A, C23A, C24A, C25A, C26A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(F14)=Sof(F13)=Sof(F15)=FVAR(1)
 Sof(F17A)=Sof(F18A)=Sof(F16A)=1-FVAR(2)
 Sof(F16)=Sof(F18)=Sof(F17)=FVAR(2)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(3)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(3)
 Sof(F11A)=Sof(F10A)=Sof(F12A)=1-FVAR(4)
 Sof(F11)=Sof(F10)=Sof(F12)=FVAR(4)
 Sof(C21A)=Sof(H21A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25C)=
 Sof(H25D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=
 Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(5)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C15(H15), C7(H7), C21(H21), C21A(H21A)
6.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C6(H6A,H6B), C28(H28A,H28B), C19(H19A,H19B),
 C12(H12A,H12B), C10(H10A,H10B), C5(H5A,H5B), C2(H2A,H2B), C20(H20A,H20B),
 C9(H9A,H9B), C29(H29A,H29B), C16(H16A,H16B), C18(H18A,H18B), C8(H8A,H8B),
 C4(H4A,H4B), C17(H17A,H17B), C22(H22A,H22B), C3(H3A,H3B), C11(H11A,H11B),
 C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C25(H25A,H25B), C26A(H26C,
 H26D), C25A(H25C,H25D), C24A(H24C,H24D), C23A(H23C,H23D), C22A(H22C,H22D)
6.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C36(H36), C40(H40), C48(H48), C52(H52), C56(H56), C34(H34),
 C44(H44), C60(H60), C50(H50), C58(H58), C42(H42)
6.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              81036
_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
;