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_7126240
_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         'C29 H54 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C61 H66 B F24 P2 Rh'
_chemical_formula_weight         1430.79
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                91.347(4)
_cell_angle_beta                 90.717(5)
_cell_angle_gamma                96.597(6)
_cell_formula_units_Z            2
_cell_length_a                   12.8015(10)
_cell_length_b                   12.9012(7)
_cell_length_c                   19.8814(9)
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    150.1(2)
_cell_measurement_theta_max      75.4890
_cell_measurement_theta_min      4.0010
_cell_volume                     3260.5(3)
_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_environment      N~2~
_diffrn_ambient_temperature      150.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_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    -10.00  31.00   1.00   10.00    --  -41.91  38.00 -60.00   41
  2  \w   -111.00 -10.00   1.00   10.00    --  -41.91 -19.00 150.00  101
  3  \w    -48.00  -7.00   1.00   10.00    --  -41.91  38.00 120.00   41
  4  \w     59.00 119.00   1.00   10.00    --   41.91 178.00  90.00   60
  5  \w     95.00 174.00   1.00   50.00    --  111.00 125.00  30.00   79
  6  \w     41.00  68.00   1.00   50.00    --  111.00 -30.00-180.00   27
  7  \w     46.00  90.00   1.00   50.00    --  111.00 -30.00   0.00   44
  8  \w     42.00  69.00   1.00   50.00    --  111.00 -45.00  60.00   27
  9  \w     38.00  66.00   1.00   50.00    --  111.00 -30.00 120.00   28
 10  \w     54.00 137.00   1.00   50.00    --  111.00 -77.00  60.00   83
 11  \w     33.00 109.00   1.00   50.00    --  111.00 -95.00   0.00   76
 12  \w     67.00  92.00   1.00   50.00    --  111.00-125.00 -60.00   25
 13  \w     45.00  90.00   1.00   50.00    --  111.00 -30.00  60.00   45
 14  \w     83.00 108.00   1.00   50.00    --  111.00-103.00 -56.00   25
 15  \w     45.00  88.00   1.00   50.00    --  111.00 -45.00 150.00   43
 16  \w   -114.00 -21.00   1.00   10.00    --  -41.91 -38.00 -90.00   93
 17  \w    -91.00 -22.00   1.00   10.00    --  -41.91 -38.00 -30.00   69
 18  \w      1.00  33.00   1.00   10.00    --   41.91 -99.00 150.00   32
 19  \w     67.00  96.00   1.00   50.00    --  111.00 -45.00 -30.00   29
 20  \w     88.00 175.00   1.00   50.00    --  111.00  30.00-150.00   87
 21  \w     60.00  88.00   1.00   50.00    --  111.00 -45.00-120.00   28
 22  \w     77.00 115.00   1.00   50.00    --  111.00-125.00-120.00   38
 23  \w     96.00 125.00   1.00   50.00    --  111.00 125.00  60.00   29
 24  \w    151.00 176.00   1.00   50.00    --  111.00 125.00  60.00   25
 25  \w     92.00 118.00   1.00   50.00    --  111.00-125.00 150.00   26
 26  \w     53.00  80.00   1.00   50.00    --  111.00 -30.00-150.00   27
 27  \w     53.00  80.00   1.00   50.00    --  111.00-125.00 -90.00   27
 28  \w     97.00 166.00   1.00   50.00    --  111.00 125.00 150.00   69
 29  \w     93.00 118.00   1.00   50.00    --  111.00-125.00 -60.00   25
 30  \w     40.00 115.00   1.00   50.00    --  111.00 -15.00-120.00   75
 31  \w     36.00  65.00   1.00   10.00    --   41.91 -77.00  90.00   29
 32  \w     85.00 126.00   1.00   10.00    --   41.91 178.00 -30.00   41
 33  \w     54.00  83.00   1.00   50.00    --  111.00 -30.00  30.00   29
 34  \w     37.00  81.00   1.00   50.00    --  111.00 -30.00-150.00   44
 35  \w     61.00  88.00   1.00   50.00    --  111.00-125.00   0.00   27
 36  \w     93.00 118.00   1.00   50.00    --  111.00-125.00   0.00   25
 37  \w     46.00  73.00   1.00   50.00    --  111.00 -30.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1089569000
_diffrn_orient_matrix_UB_12      -0.0637714000
_diffrn_orient_matrix_UB_13      0.0045060000
_diffrn_orient_matrix_UB_21      0.0059009000
_diffrn_orient_matrix_UB_22      0.0111894000
_diffrn_orient_matrix_UB_23      0.0773128000
_diffrn_orient_matrix_UB_31      -0.0526587000
_diffrn_orient_matrix_UB_32      0.1013272000
_diffrn_orient_matrix_UB_33      -0.0033920000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29822
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.069
_diffrn_reflns_theta_min         4.449
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.532
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81293
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.271
_refine_diff_density_min         -1.750
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     971
_refine_ls_number_reflns         29822
_refine_ls_number_restraints     785
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.1003
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2905
_refine_ls_wR_factor_ref         0.3209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21988
_reflns_number_total             29822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01140a3.cif
_cod_data_source_block           260amm19twin
_cod_depositor_comments
'Adding full bibliography for 7126239--7126241.cif.'
_cod_database_code               7126240
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 Rh1 B1 F24 P2'
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.553
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.636(5)
 0.364(5)
2. 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
3. Restrained distances
 F11-F10 \\sim F11-F12 \\sim F10-F12 \\sim F11A-F10A \\sim F11A-F12A \\sim
F10A-F12A
 with sigma of 0.04
 C45-F11 \\sim C45-F10 \\sim C45-F12 \\sim C45-F11A \\sim C45-F10A \\sim
C45-F12A
 with sigma of 0.02
 F23-F24 \\sim F23-F22 \\sim F24-F22 \\sim F23A-F24A \\sim F23A-F22A \\sim
F24A-F22A
 with sigma of 0.04
 C61-F23 \\sim C61-F24 \\sim C61-F22 \\sim C61-F23A \\sim C61-F24A \\sim
C61-F22A
 with sigma of 0.02
 F6-F4 \\sim F6-F5 \\sim F4-F5 \\sim F6A-F4A \\sim F6A-F5A \\sim F4A-F5A
 with sigma of 0.04
 C37-F6 \\sim C37-F4 \\sim C37-F5 \\sim C37-F6A \\sim C37-F4A \\sim C37-F5A
 with sigma of 0.02
 F8-F9 \\sim F8-F7 \\sim F9-F7 \\sim F8A-F9A \\sim F8A-F7A \\sim F9A-F7A
 with sigma of 0.04
 C44-F8 \\sim C44-F9 \\sim C44-F7 \\sim C44-F8A \\sim C44-F9A \\sim C44-F7A
 with sigma of 0.02
 F18-F17 \\sim F18-F16 \\sim F17-F16 \\sim F18A-F17A \\sim F18A-F16A \\sim
F17A-F16A
 with sigma of 0.04
 C53-F18 \\sim C53-F17 \\sim C53-F16 \\sim C53-F18A \\sim C53-F17A \\sim
C53-F16A
 with sigma of 0.02
 Rh1-C1A \\sim Rh1-C1
 with sigma of 0.02
 Rh1-C2A \\sim Rh1-C2
 with sigma of 0.02
 C1A-C2A \\sim C1-C2
 with sigma of 0.02
 Rh1-C3A \\sim Rh1-C3
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C45 \\sim F10A \\sim F11A \\sim F12A \\sim F10 \\sim F11 \\sim F12: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C61 \\sim F22A \\sim F23A \\sim F24A \\sim F22 \\sim F23 \\sim F24: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C37 \\sim F4A \\sim F5A \\sim F6A \\sim F4 \\sim F5 \\sim F6: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C44 \\sim F7A \\sim F8A \\sim F9A \\sim F7 \\sim F8 \\sim F9: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C53 \\sim F16A \\sim F17A \\sim F18A \\sim F16 \\sim F17 \\sim F18: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
C1A \\sim C2A \\sim C3A \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C45, F10A, F11A, F12A, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61, F22A, F23A, F24A, F22, F23, F24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, F4A, F5A, F6A, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, F7A, F8A, F9A, F7, F8, F9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, F16A, F17A, F18A, F16, F17, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(2)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(5)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(5)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=1-FVAR(6)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=
 FVAR(6)
7.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C18(H18), C24(H24)
7.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B)
7.c Me refined with riding coordinates:
 C3A(H3AA,H3AB,H3AC), C3(H3A,H3B,H3C)
7.d Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C31(H31), C33(H33), C35(H35), C39(H39), C41(H41), C43(H43),
 C47(H47), C49(H49), C51(H51), C55(H55), C57(H57), C59(H59), C2(H2)
7.e X=CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1(H1A,H1B)
;
_shelx_res_checksum              55909
_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 1.617
_oxdiff_exptl_absorpt_empirical_full_min 0.715