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_7123389
_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_absolute_configuration unk
_chemical_formula_moiety         'C69 H56 Cl N O3 Os P3, 0.25(C H2 Cl2), B F4'
_chemical_formula_sum            'C69.25 H56.5 B Cl1.5 F4 N O3 Os P3'
_chemical_formula_weight         1373.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-11
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.604(3)
_cell_length_b                   13.735(3)
_cell_length_c                   34.365(7)
_cell_measurement_reflns_used    43792
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.17
_cell_measurement_theta_min      5.99
_cell_volume                     6421(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            41679
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.995
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.5416
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2762
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.152
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 4420 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11264
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+15.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                10701
_reflns_number_total             11264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02594d2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C69.25 H56.50 B Cl1.50 F4 N O3 Os P3'
_cod_database_code               7123389
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C1S-Cl1A
 1.77 with sigma of 0.03
 C1S-Cl1B
 1.77 with sigma of 0.03
 Cl1A-Cl1B
 2.89 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: C1S(0.25) H1SA(0.25) H1SB(0.25) Cl1B(0.25) Cl1A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C0AA(H0AA), C010(H010), C011(H011), C012(H012),
 C013(H013), C1AA(H1AA), C014(H014), C16(H16), C18(H18), C20(H20), C12(H12),
 C23(H23), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C38(H38), C39(H39),
  C15(H15), C43(H43), C44(H44), C11(H11), C47(H47), C48(H48), C49(H49),
 C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C13(H13), C57(H57), C59(H59),
  C60(H60), C14(H14), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67),
 C68(H68), C71(H71), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
  C80(H80)
;
_shelx_res_checksum              80276
_shelx_hkl_checksum              93724
_olex2_submission_special_instructions 'No special instructions were received'