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_1568946
_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
'C81 H64 Cl2 Os P4, 2(Cl), 2(C H2 Cl2), 2(H2 O)'
_chemical_formula_sum            'C83 H72 Cl8 O2 Os P4'
_chemical_formula_weight         1699.08
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-21
_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                108.2270(10)
_cell_angle_beta                 96.2310(10)
_cell_angle_gamma                98.1170(10)
_cell_formula_units_Z            2
_cell_length_a                   12.70740(10)
_cell_length_b                   15.86420(10)
_cell_length_c                   19.70260(10)
_cell_measurement_reflns_used    76084
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      31.3910
_cell_measurement_theta_min      1.9930
_cell_volume                     3685.24(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.878
_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     20.00  80.00   0.50   15.00    --   13.19-144.00  69.00  120
  2  \w     11.00  70.00   0.50   15.00    --   13.19-127.00-121.00  118
  3  \w    -55.00   2.00   0.50   15.00    --  -11.78 -19.00 150.00  114
  4  \w    -43.00 -18.00   0.50   15.00    --  -11.78  77.00  90.00   50
  5  \w    -85.00  16.00   0.50   15.00    --  -11.78 -77.00   0.00  202
  6  \w    -13.00  30.00   0.50   15.00    --  -11.78 -99.00-120.00   86
  7  \w    -93.00 -68.00   0.50   15.00    --  -11.78 -19.00 150.00   50
  8  \w      5.00  63.00   0.50   15.00    --  -11.78  77.00  90.00  116
  9  \w    -85.00  19.00   0.50   15.00    --  -11.78 -77.00-180.00  208
 10  \w    -39.00 -13.00   0.50   15.00    --  -11.78  77.00-180.00   52
 11  \w      7.00  63.00   0.50   15.00    --  -11.78  77.00-180.00  112
 12  \w     14.00  55.00   0.50   15.00    --   13.19 -99.00-180.00   82
 13  \w    -26.00   5.00   0.50   15.00    --   13.19 -99.00-180.00   62
 14  \w    -68.00  -6.00   0.50   15.00    --   13.19 -19.00  90.00  124
 15  \w    -10.00  88.00   0.50   15.00    --   13.19  57.00  60.00  196
 16  \w      0.00  62.00   0.50   15.00    --   13.19-112.00  23.01  124
 17  \w     33.00  87.00   0.50   15.00    --   13.19  57.00-180.00  108
 18  \w    -11.00  30.00   0.50   15.00    --   13.19  57.00-180.00   82
 19  \w     -4.00  59.00   0.50   15.00    --   13.19-107.00 -34.44  126
 20  \w    -68.00  -5.00   0.50   15.00    --   13.19 -19.00 -90.00  126
;
_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      0.0235734000
_diffrn_orient_matrix_UB_12      -0.0388717000
_diffrn_orient_matrix_UB_13      -0.0040023000
_diffrn_orient_matrix_UB_21      0.0149230000
_diffrn_orient_matrix_UB_22      0.0135325000
_diffrn_orient_matrix_UB_23      0.0381292000
_diffrn_orient_matrix_UB_31      -0.0498673000
_diffrn_orient_matrix_UB_32      -0.0245078000
_diffrn_orient_matrix_UB_33      0.0023705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            116361
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.217
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.531
_exptl_crystal_description       needle
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         21032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0210P)^2^+6.5020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19318
_reflns_number_total             21032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01491f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1568944--1568946.cif.'
_cod_database_code               1568946
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C83 H72 Cl8 O2 Os1 P4'
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1.a Free rotating group:
 O00E(H00A,H00B), O00F(H00C,H00D)
1.b Secondary CH2 refined with riding coordinates:
 C02N(H02N,H02Q), C02Q(H02R,H02S)
1.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C6(H6), C00M(H00M), C1(H1), C00P(H00P), C00Q(H00Q),
 C9(H9), C00U(H00U), C00X(H00X), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
  C014(H014), C3(H3), C016(H016), C018(H018), C019(H019), C01B(H01B),
 C01F(H01F), C01G(H01G), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01X(H01X), C01Y(H01Y),
 C01Z(H01Z), C020(H020), C021(H021), C022(H022), C023(H023), C024(H024),
 C025(H025), C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
 C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M),
 C02O(H02O), C02P(H02P)
;
_shelx_res_checksum              10486
_shelx_hkl_checksum              66982
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.781