(η4-Tetrafluorobenzobarrelene)-η1-((tri-4-fluorophenyl)phosphine)-η1-(2-phenylphenyl)rhodium(I): A Catalyst for the Living Polymerization of Phenylacetylenes
Sheng Loong Tan, Nicholas; Nealon, Gareth L.; Moggach, Stephen A.; Lynam, Jason M.; Ogden, Mark I.; Massi, Massimiliano; Lowe, Andrew B.; Macromolecules  (2021) –; doi:10.1021/acs.macromol.1c00906

data_1563710
_publ_section_title
;
 (\h4-Tetrafluorobenzobarrelene)-\h1-((tri-4-fluorophenyl)phosphine)-\h1-(2-phenylphenyl)rhodium(I):
 A Catalyst for the Living Polymerization of Phenylacetylenes
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.1c00906
_journal_year                    2021
_chemical_formula_moiety         'C42 H27 F7 P Rh'
_chemical_formula_sum            'C42 H27 F7 P Rh'
_chemical_formula_weight         798.51
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.3019(3)
_cell_length_b                   10.31750(10)
_cell_length_c                   25.1310(4)
_cell_measurement_reflns_used    36332
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.4450
_cell_measurement_theta_min      3.3520
_cell_volume                     6796.55(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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    -73.00  27.00   0.50    0.10    --  -46.20  87.00 161.00  200
  2  \w    -25.00  73.00   0.50    0.10    --   46.20 -87.00  43.00  196
  3  \w   -175.00 -79.00   0.50    0.50    -- -102.41 -87.00  43.00  192
  4  \w   -129.00 -30.00   0.50    0.50    -- -102.41  87.00 161.00  198
  5  \w     79.00 175.00   0.50    0.50    --  102.41  87.00 161.00  192
  6  \w     30.00 130.00   0.50    0.50    --  102.41 -87.00  43.00  200
  7  \w   -118.00 -73.00   0.50    0.10    --  -46.20-125.00-180.00   90
  8  \w   -118.00 -73.00   0.50    0.10    --  -46.20-125.00 -90.00   90
  9  \w   -118.00 -23.00   0.50    0.10    --  -46.20 -77.00  60.00  190
 10  \w     24.00 118.00   0.50    0.10    --   46.20  77.00-150.00  188
 11  \w     34.00 119.00   0.50    0.10    --   46.20  38.00 -90.00  170
 12  \w   -175.00 -83.00   0.50    0.50    -- -102.41 -94.00  90.00  184
 13  \w   -116.00 -27.00   0.50    0.50    -- -102.41  15.00-180.00  178
 14  \w   -174.00 -90.00   0.50    0.50    -- -102.41 -45.00  90.00  168
 15  \w   -177.00 -90.00   0.50    0.50    -- -102.41 -30.00 150.00  174
 16  \w   -177.00 -90.00   0.50    0.50    -- -102.41 -30.00 -60.00  174
 17  \w   -174.00 -90.00   0.50    0.50    -- -102.41 -45.00 120.00  168
 18  \w   -115.00 -27.00   0.50    0.50    -- -102.41  30.00-180.00  176
 19  \w   -175.00 -83.00   0.50    0.50    -- -102.41 -94.00  30.00  184
 20  \w   -175.00 -83.00   0.50    0.50    -- -102.41 -94.00 150.00  184
 21  \w     30.00 105.00   0.50    0.50    --  102.41 -94.00  30.00  150
 22  \w     90.00 174.00   0.50    0.50    --  102.41  45.00 120.00  168
 23  \w     90.00 174.00   0.50    0.50    --  102.41  45.00 -60.00  168
 24  \w     30.00 111.00   0.50    0.50    --  102.41-125.00  90.00  162
 25  \w     90.00 177.00   0.50    0.50    --  102.41  30.00-120.00  174
 26  \w     24.00 118.00   0.50    0.10    --   46.20  77.00 -30.00  188
 27  \w     24.00 118.00   0.50    0.10    --   46.20  77.00  60.00  188
 28  \w     31.00 118.00   0.50    0.10    --   46.20  57.00 -60.00  174
 29  \w     31.00 118.00   0.50    0.10    --   46.20  57.00 150.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0558612000
_diffrn_orient_matrix_UB_12      0.0287720000
_diffrn_orient_matrix_UB_13      -0.0100296000
_diffrn_orient_matrix_UB_21      0.0031151000
_diffrn_orient_matrix_UB_22      -0.1302384000
_diffrn_orient_matrix_UB_23      -0.0294394000
_diffrn_orient_matrix_UB_31      -0.0179073000
_diffrn_orient_matrix_UB_32      0.0673280000
_diffrn_orient_matrix_UB_33      -0.0530583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60027
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.623
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.115
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       plate
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.841
_refine_diff_density_min         -1.925
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0559P)^2^+22.6365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6279
_reflns_number_total             6909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00906_si_002.cif
_cod_data_source_block           mxmsteve
_cod_database_code               1563710
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Rh1 P1 F7 C42 H25'
_chemical_oxdiff_usercomment     'Mark Ogden for Max Massi'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C00B(H00B), C00G(H00G), C00H(H00H), C00K(H00K), C00O(H00O), C00W(H00W)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00I(H00I), C00M(H00M), C00P(H00P), C00R(H00R), C00T(H00T),
 C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C013(H013), C016(H016),
 C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C),
 C01D(H01D), C01E(H01E), C01F(H01F)
;
_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 2.402
_oxdiff_exptl_absorpt_empirical_full_min 0.665