Synthesis and Characterization of Metallapentalenoxazetes from the [2+2] Cycloaddition of Metallapentalynes with Nitrosoarenes
Deng, Zhihong; Zhu, Congqing; Hua, Yuhui; HE, Guomei; Guo, Ying; Lu, Ruqiang; Cao, Xiaoyu; Chen, Jiangxi; Xia, Haiping; Chemical Communications  (2019) –; doi:10.1039/C9CC02594D

data_7123390
_publ_section_title
;
 Synthesis and Characterization of Metallapentalenoxazetes from the [2+2]
 Cycloaddition of Metallapentalynes with Nitrosoarenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02594D
_journal_year                    2019
_chemical_formula_moiety         'C74 H62 Cl N O5 Os P3, 3(C H2 Cl2), B F4'
_chemical_formula_sum            'C77 H68 B Cl7 F4 N O5 Os P3'
_chemical_formula_weight         1705.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-11 deposited with the CCDC.    2019-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.4950(10)
_cell_angle_beta                 103.8640(10)
_cell_angle_gamma                101.6860(10)
_cell_formula_units_Z            2
_cell_length_a                   12.28710(10)
_cell_length_b                   14.71150(10)
_cell_length_c                   21.50510(10)
_cell_measurement_reflns_used    30593
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.9580
_cell_measurement_theta_min      3.7940
_cell_volume                     3671.23(5)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -118.00 -26.00   0.50    0.08    --  -46.75 -72.00 -42.00  184
  2  \w     26.00 109.00   0.50    0.08    --   46.75  72.00  87.00  166
  3  \w    -24.00   2.00   0.50    0.08    --   46.75 -72.00 -42.00   52
  4  \w     37.00  63.00   0.50    0.08    --   46.75 -72.00 -42.00   52
  5  \w    -99.00 -73.00   0.50    0.24    --  -88.50 -72.00 -42.00   52
  6  \w     88.00 177.00   0.50    0.24    --  110.00  72.00  87.00  178
  7  \w     97.00 132.00   0.50    0.24    --  110.00 -72.00 -42.00   70
  8  \w     47.00  83.00   0.50    0.24    --  110.00 -72.00 -42.00   72
  9  \w    -68.00  -1.00   0.50    0.08    --  -46.75  72.00  87.00  134
 10  \w    -60.00 -13.00   0.50    0.08    --  -46.75  57.00-150.00   94
 11  \w    -90.00 -24.00   0.50    0.08    --  -46.75 125.00  90.00  132
 12  \w     -2.00  26.00   0.50    0.08    --  -46.75  57.00-150.00   56
 13  \w   -119.00 -94.00   0.50    0.08    --  -46.75-125.00-180.00   50
 14  \w     31.00  93.00   0.50    0.08    --   46.75-125.00 -30.00  124
 15  \w   -124.00 -83.00   0.50    0.24    --  -88.50 -99.00  60.00   82
 16  \w   -156.00 -85.00   0.50    0.24    --  -88.50 -99.00  30.00  142
 17  \w   -153.00-119.00   0.50    0.24    --  -88.50-125.00 -60.00   68
 18  \w    -67.00 -41.00   0.50    0.24    --  -88.50  72.00  87.00   52
 19  \w   -117.00 -74.00   0.50    0.24    --  -88.50 -37.00-120.00   86
 20  \w   -100.00 -73.00   0.50    0.24    --  -88.50-125.00 -60.00   54
 21  \w     53.00 106.00   0.50    0.24    --  110.00-125.00 -60.00  106
 22  \w     81.00 117.00   0.50    0.24    --  110.00-125.00-150.00   72
 23  \w     94.00 132.00   0.50    0.24    --  110.00 -77.00  90.00   76
 24  \w    141.00 168.00   0.50    0.24    --  110.00  57.00-150.00   54
 25  \w     98.00 140.00   0.50    0.24    --  110.00  57.00-150.00   84
 26  \w     84.00 126.00   0.50    0.24    --  110.00 -19.00  30.00   84
 27  \w     92.00 170.00   0.50    0.24    --  110.00 125.00   0.00  156
 28  \w     35.00  72.00   0.50    0.24    --  110.00 -19.00  30.00   74
 29  \w    108.00 160.00   0.50    0.24    --  110.00  19.00   0.00  104
 30  \w     38.00 108.00   0.50    0.24    --  110.00 -99.00  30.00  140
 31  \w     56.00 110.00   0.50    0.24    --  110.00 -99.00 -30.00  108
 32  \w     85.00 110.00   0.50    0.24    --  110.00 -99.00-180.00   50
 33  \w     98.00 135.00   0.50    0.24    --  110.00 125.00-120.00   74
 34  \w     46.00  81.00   0.50    0.24    --  110.00 -77.00  90.00   70
 35  \w     38.00 116.00   0.50    0.24    --  110.00-125.00-180.00  156
 36  \w    152.00 177.00   0.50    0.24    --  110.00  57.00-180.00   50
 37  \w     47.00  75.00   0.50    0.24    --  110.00 -37.00-120.00   56
 38  \w    100.00 125.00   0.50    0.24    --  110.00 -37.00-120.00   50
 39  \w     95.00 139.00   0.50    0.24    --  110.00  57.00-180.00   88
 40  \w     45.00  71.00   0.50    0.24    --  110.00 -99.00-180.00   52
;
_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      0.0242651000
_diffrn_orient_matrix_UB_12      -0.0615921000
_diffrn_orient_matrix_UB_13      0.0548668000
_diffrn_orient_matrix_UB_21      -0.1026372000
_diffrn_orient_matrix_UB_22      0.0212741000
_diffrn_orient_matrix_UB_23      0.0230119000
_diffrn_orient_matrix_UB_31      -0.0802275000
_diffrn_orient_matrix_UB_32      -0.0856890000
_diffrn_orient_matrix_UB_33      -0.0444714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41192
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        64.999
_diffrn_reflns_theta_max         64.999
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58433
_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            'metallic light orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.703
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         12474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+12.7198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11855
_reflns_number_total             12474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02594d2.cif
_cod_data_source_block           dzh-20180726-1
_cod_database_code               7123390
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C02K(H02K,H02M), C02Q(H02Q,H02R), C02R(H02S,H02T)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C00T(H00T), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C010(H010), C19(H19), C012(H012), C20(H20), C016(H016), C017(H017), C01A(H01A),
  C18(H18), C16(H16), C01F(H01F), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01O(H01O), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T),
 C01U(H01U), C01V(H01V), C01W(H01W), C17(H17), C01Z(H01Z), C020(H020),
 C021(H021), C022(H022), C023(H023), C024(H024), C026(H026), C029(H029),
 C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F),
 C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02L(H02L), C02N(H02N),
 C02O(H02O), C02P(H02P)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              35014
_shelx_hkl_checksum              85082
_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 1.990
_oxdiff_exptl_absorpt_empirical_full_min 0.637