Reshaping aromatic frameworks: expansion of aromatic system drives metallabenzenoids to metallapentalenes.
Li, Qian; Fei, Jiawei; Ruan, Kaidong; Hua, Yuhui; Chen, Dafa; Luo, Ming; Xia, Haiping; Chemical science 14 (2023) 5672–5680; doi:10.1039/d3sc01491f

data_1568945
_publ_section_title
;
 Reshaping aromatic frameworks: expansion of aromatic system drives
 metallabenzenoids to metallapentalenes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              5672
_journal_page_last               5680
_journal_paper_doi               10.1039/d3sc01491f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C63 H52 Cl2 Os P3, C H2 Cl2, B F4'
_chemical_formula_sum            'C64 H54 B Cl4 F4 Os P3'
_chemical_formula_weight         1334.79
_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             2022-09-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-09-23 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                93.9940(10)
_cell_angle_beta                 94.966(2)
_cell_angle_gamma                95.826(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1361(2)
_cell_length_b                   12.2229(2)
_cell_length_c                   22.8285(4)
_cell_measurement_reflns_used    20513
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      73.8700
_cell_measurement_theta_min      3.6510
_cell_volume                     2794.32(9)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_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    -24.00  36.00   0.50    1.00    --  -43.10  19.00 -60.00  120
  2  \w    -25.00  38.00   0.50    1.00    --  -43.10  19.00-150.00  126
  3  \w    -25.00  10.00   0.50    1.00    --  -43.10  19.00 -90.00   70
  4  \w    -44.00 -17.00   0.50    1.60    --  -90.25  45.00   0.00   54
  5  \w    -50.00 -18.00   0.50    1.60    --  -90.25  45.00 -30.00   64
  6  \w    -51.00 -26.00   0.50    1.60    --  -90.25  45.00-120.00   50
  7  \w    -50.00 -16.00   0.50    1.60    --  -90.25  45.00-150.00   68
  8  \w    -87.00 -60.00   0.50    1.60    --  -90.25 148.00 -79.00   54
  9  \w   -105.00 -66.00   0.50    1.00    --  -43.10 148.00 -79.00   78
 10  \w    -67.00 -41.00   0.50    1.60    --  -90.25 125.00  60.00   52
 11  \w    -77.00 -52.00   0.50    1.60    --  -90.25 124.00 115.00   50
 12  \w    -87.00 -25.00   0.50    1.00    --  -43.10 124.00 115.00  124
 13  \w    -71.00 -16.00   0.50    1.60    --  -90.25  61.00 150.00  110
 14  \w    -45.00 -13.00   0.50    1.60    --  -90.25  45.00  90.00   64
 15  \w    -98.00 -72.00   0.50    1.00    --  -43.10-124.00  36.00   52
 16  \w   -104.00 -73.00   0.50    1.00    --  -43.10-125.00  90.00   62
 17  \w   -135.00 -83.00   0.50    1.60    --  -90.25-124.00  36.00  104
 18  \w   -110.00 -60.00   0.50    1.00    --  -43.10-148.00-128.00  100
 19  \w     36.00 117.00   0.50    1.00    --   43.10  77.00 -60.00  162
 20  \w     77.00 130.00   0.50    1.60    --  107.76 148.00 -79.00  106
 21  \w     92.00 123.00   0.50    1.60    --  107.76 125.00 -30.00   62
 22  \w    145.00 171.00   0.50    1.60    --  107.76 125.00  30.00   52
 23  \w    125.00 172.00   0.50    1.60    --  107.76  61.00 120.00   94
 24  \w    111.00 136.00   0.50    1.60    --  107.76 124.00 115.00   50
 25  \w     93.00 153.00   0.50    1.60    --  107.76 125.00  60.00  120
 26  \w     84.00 110.00   0.50    1.60    --  107.76  30.00   0.00   52
 27  \w    118.00 165.00   0.50    1.60    --  107.76  30.00   0.00   94
 28  \w     95.00 121.00   0.50    1.60    --  107.76 125.00  30.00   52
 29  \w     92.00 117.00   0.50    1.60    --  107.76  61.00 120.00   50
 30  \w     35.00  66.00   0.50    1.60    --  107.76 -61.00  60.00   62
 31  \w     50.00 105.00   0.50    1.60    --  107.76 -77.00  60.00  110
 32  \w     70.00 110.00   0.50    1.60    --  107.76-124.00  36.00   80
 33  \w     78.00 103.00   0.50    1.60    --  107.76 -77.00 -30.00   50
 34  \w     70.00 104.00   0.50    1.60    --  107.76 -94.00 -60.00   68
 35  \w     88.00 133.00   0.50    1.60    --  107.76-148.00-128.00   90
 36  \w     69.00  94.00   0.50    1.00    --   43.10-148.00-128.00   50
 37  \w     44.00  73.00   0.50    1.60    --  107.76 -77.00 -30.00   58
 38  \w     56.00 116.00   0.50    1.60    --  107.76-125.00 -30.00  120
 39  \w     72.00 106.00   0.50    1.60    --  107.76 -94.00  60.00   68
 40  \w     41.00  66.00   0.50    1.60    --  107.76 -61.00 -30.00   50
 41  \w     33.00  69.00   0.50    1.60    --  107.76 -61.00   0.00   72
 42  \w     35.00 115.00   0.50    1.60    --  107.76-125.00  90.00  160
 43  \w     33.00 108.00   0.50    1.60    --  107.76 -94.00 150.00  150
 44  \w     31.00  69.00   0.50    1.00    --   43.10-124.00  36.00   76
 45  \w     34.00 110.50   0.50    1.60    --  107.76-125.00 -90.00  153
 46  \w     40.00  65.00   0.50    1.60    --  107.76 -61.00-180.00   50
 47  \w     36.00  71.00   0.50    1.60    --  107.76 -61.00-120.00   70
 48  \w     41.00 100.00   0.50    1.60    --  107.76-125.00-120.00  118
 49  \w     82.00 176.00   0.50    1.60    --  107.76  45.00 -90.00  188
 50  \w    107.00 133.00   0.50    1.60    --  107.76 125.00-150.00   52
 51  \w     93.00 127.00   0.50    1.60    --  107.76 125.00-180.00   68
 52  \w   -129.00-104.00   0.50    1.60    --  -90.25-148.00-128.00   50
 53  \w   -165.00 -85.00   0.50    1.60    --  -90.25 -45.00  90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1429968000
_diffrn_orient_matrix_UB_12      -0.0100090000
_diffrn_orient_matrix_UB_13      -0.0161204000
_diffrn_orient_matrix_UB_21      -0.0474034000
_diffrn_orient_matrix_UB_22      0.0034117000
_diffrn_orient_matrix_UB_23      -0.0657482000
_diffrn_orient_matrix_UB_31      0.0292416000
_diffrn_orient_matrix_UB_32      0.1266516000
_diffrn_orient_matrix_UB_33      0.0058938000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35168
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.594
_diffrn_reflns_theta_min         3.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.331
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.392
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.074
_refine_diff_density_max         3.079
_refine_diff_density_min         -2.037
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+15.4014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1097
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10425
_reflns_number_total             11065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01491f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1568944--1568946.cif.'
_cod_database_code               1568945
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C64 H54 B Cl4 F4 Os P3'
_olex2_refinement_description
;
1. Others
 Fixed Sof: F022(0.75) F026(0.25)
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C3(H3A,H3B), C025(H02A,H02B)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C1(H1), C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00W(H00W),
  C00X(H00X), C00Y(H00Y), C7(H7), C011(H011), C012(H012), C015(H015),
 C016(H016), C018(H018), C019(H019), C01A(H01A), C6(H6), C01C(H01C), C01D(H01D),
  C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y),
 C01Z(H01Z), C020(H020), C021(H021), C023(H023)
;
_shelx_res_checksum              46288
_shelx_hkl_checksum              54274
_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 3.893
_oxdiff_exptl_absorpt_empirical_full_min 0.428