Benzyne addition to a metal-carbon multiple bond.
Barnett, Harrison J.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9383–9387; doi:10.1039/d1dt01402a

data_7707720
_publ_section_title
;
 Benzyne addition to a metal-carbon multiple bond.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9383
_journal_page_last               9387
_journal_paper_doi               10.1039/d1dt01402a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C60 H50.5 Cl3.5 P4 Rh2'
_chemical_formula_sum            'C60 H50.5 Cl3.5 P4 Rh2'
_chemical_formula_weight         1225.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-10 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.99510(10)
_cell_length_b                   14.99510(10)
_cell_length_c                   26.1521(4)
_cell_measurement_reflns_used    6864
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.7770
_cell_measurement_theta_min      4.1720
_cell_volume                     5880.38(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.981
_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    -52.00  22.00   1.00    1.00    --  -36.03  19.00  90.00   74
  2  \w     40.00  78.00   1.00    1.00    --   36.03-125.00  60.00   38
  3  \w     56.00  90.00   1.00    1.00    --  105.15 -95.00 -30.00   34
  4  \w    108.00 173.00   1.00    1.00    --  105.15 111.00  60.00   65
  5  \w    104.00 174.00   1.00    1.00    --  105.15 111.00 -30.00   70
  6  \w    106.00 175.00   1.00    1.00    --  105.15 111.00   0.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143410000
_diffrn_orient_matrix_UB_12      0.0228663000
_diffrn_orient_matrix_UB_13      -0.0567924000
_diffrn_orient_matrix_UB_21      -0.0784477000
_diffrn_orient_matrix_UB_22      0.0661886000
_diffrn_orient_matrix_UB_23      0.0023963000
_diffrn_orient_matrix_UB_31      0.0648157000
_diffrn_orient_matrix_UB_32      0.0751768000
_diffrn_orient_matrix_UB_33      0.0154066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10253
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.952
_diffrn_reflns_theta_min         4.169
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.305
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 2173 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5538
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0602P)^2^+2.7805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                5367
_reflns_number_total             5538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01402a2.cif
_cod_data_source_block           hb_1285_9_1_scale
_cod_depositor_comments
'Adding full bibliography for 7707720--7707721.cif.'
_cod_original_cell_volume        5880.38(12)
_cod_original_formula_sum        'C60 H50.50 Cl3.50 P4 Rh2'
_cod_database_code               7707720
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C7, C5, C3, C6, C4, C2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C10, C8, C12, C13, C11, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Rh1, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C7 \\sim C5 \\sim C3 \\sim C6 \\sim C4 \\sim C2: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C10 \\sim C8 \\sim C12 \\sim C13 \\sim C11 \\sim C9: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl3(0.25) C7(0.5) H7(0.5) C6(0.5) H6(0.5) C5(0.5) H5(0.5) C4(0.5)
 H4(0.5) C3(0.5) C2(0.5) C8(0.25) C13(0.25) H13(0.25) C12(0.25) H12(0.25)
 C11(0.25) H11(0.25) C10(0.25) H10(0.25) C9(0.25) H9(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C44(H44), C53(H53), C54(H54), C36(H36),
 C13(H13), C12(H12), C11(H11), C10(H10), C9(H9), C46(H46), C32(H32), C43(H43),
 C22(H22), C56(H56), C45(H45), C23(H23), C42(H42), C33(H33), C52(H52), C26(H26),
  C34(H34), C25(H25), C55(H55), C24(H24), C35(H35)
5.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C3,C2), C8(C13,C12,C11,C10,C9)
;
_shelx_res_checksum              9543
_ins_header
;
TITL HB_1285_9_1_scale in P4(1)2(1)2 
REM P4(1)2(1)2 (#92 in standard setting)
CELL 1.54184  14.995112  14.995112  26.152081  90.0000  90.0000  90.0000
ZERR    4.00   0.000118   0.000118   0.000369   0.0000   0.0000   0.0000
LATT -1
SYMM -x,-y, z+1/2 
SYMM -y+1/2, x+1/2, z+1/4 
SYMM  y+1/2,-x+1/2, z+3/4 
SYMM -x+1/2, y+1/2,-z+1/4 
SYMM  x+1/2,-y+1/2,-z+3/4 
SYMM  y, x,-z 
SYMM -y,-x,-z+1/2 
SFAC C H P Cl Rh
UNIT 240.00 200.00 16.00 12.00 8.00
TREF
HKLF 4
END
;
_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 1.172
_oxdiff_exptl_absorpt_empirical_full_min 0.663