Fused Metallacyclopropenes from Alkynylphenols
Fu, Bingjie; Bai, Wei; Zhao, Yue; Yang, Li; Jiang, Wen-Feng; Chemical Communications  (2023) –; doi:10.1039/D3CC03084A

data_7132040
_publ_section_title
;
 Fused Metallacyclopropenes from Alkynylphenols
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03084A
_journal_year                    2023
_chemical_formula_moiety
'C48 H43 Cl2 O3 Os P2, 0.695(C H2 Cl2)'
_chemical_formula_sum            'C48.5 H44 Cl3 O3 Os P2'
_chemical_formula_weight         1033.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-20 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.7310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5392(5)
_cell_length_b                   13.2966(3)
_cell_length_c                   30.5699(8)
_cell_measurement_reflns_used    9744
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      74.484
_cell_measurement_theta_min      3.298
_cell_volume                     8629.2(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80741
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.588
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_min         2.081
_diffrn_source_current           0.95
_diffrn_source_power             0.0475
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.323
_exptl_absorpt_correction_T_max  0.0872
_exptl_absorpt_correction_T_min  0.0077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1223 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.0883.
The \l/2 correction factor is Not present.
;
_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    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.830
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         15233
_refine_ls_number_restraints     2003
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1018P)^2^+4.2408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14304
_reflns_number_total             15233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03084a2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C97 H88 Cl6 O6 Os2 P4'
_cod_original_formula_weight         2066.65
_cod_original_formula_moiety
'2(C48 H43 Cl2 O3 Os P2), C H2 Cl2, 0.39[CH2Cl2]'
_cod_original_formula_units_Z            4
_cod_database_code               7132040
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.435
_shelx_estimated_absorpt_t_min   0.368
_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
 C54-C53
 1.5 with sigma of 0.001
 C8-C1
 1.492 with sigma of 0.001
 C8-C1 = C54-C53
 1.5 with sigma of 0.001
 C97-Cl5
 1.75 with sigma of 0.001
3. Rigid bond restraints
 Cl5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C91 \\sim C73 \\sim C78 \\sim C54 \\sim C79 \\sim C67 \\sim C56 \\sim C55 \\sim
C53 \\sim C61 \\sim C74 \\sim C85 \\sim C68 \\sim C62 \\sim C58 \\sim C81 \\sim
C57 \\sim C60 \\sim C80 \\sim C92 \\sim C77 \\sim C94 \\sim C90 \\sim C84 \\sim
C87 \\sim C51 \\sim C66 \\sim C70 \\sim C82 \\sim C69 \\sim C59 \\sim C76 \\sim
C75 \\sim C96 \\sim C95 \\sim C52 \\sim C83 \\sim C63 \\sim C72 \\sim C88 \\sim
C65 \\sim C64 \\sim C93 \\sim C71 \\sim C50 \\sim C89 \\sim C86 \\sim C49 \\sim
C31 \\sim C13 \\sim C25 \\sim C24 \\sim C43 \\sim C14 \\sim C32 \\sim C7 \\sim
C42 \\sim C2 \\sim C19 \\sim C41 \\sim C15 \\sim C28 \\sim C29 \\sim C44 \\sim
C16 \\sim C48 \\sim C36 \\sim C1 \\sim C47 \\sim C18 \\sim C37 \\sim C30 \\sim
C46 \\sim C38 \\sim C35 \\sim C17 \\sim C26 \\sim C20 \\sim C8 \\sim C22 \\sim
C45 \\sim C39 \\sim C34 \\sim C23 \\sim C6 \\sim C27 \\sim C40 \\sim C3 \\sim
C33 \\sim C5 \\sim C21 \\sim C4 \\sim C9 \\sim C11 \\sim C10 \\sim C12 \\sim
C97: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
Uanis(Cl5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C51(H51a,H51b), C52(H52a,H52b), C50(H50a,H50b), C9(H9a,H9b), C11(H11a,H11b),
 C10(H10a,H10b), C97(H97a,H97b)
5.b Aromatic/amide H refined with riding coordinates:
 C78(H78), C74(H74), C68(H68), C62(H62), C58(H58), C81(H81), C57(H57),
 C60(H60), C80(H80), C92(H92), C77(H77), C94(H94), C90(H90), C84(H84), C87(H87),
  C66(H66), C70(H70), C82(H82), C69(H69), C59(H59), C76(H76), C75(H75),
 C96(H96), C95(H95), C83(H83), C63(H63), C72(H72), C88(H88), C65(H65), C64(H64),
  C93(H93), C71(H71), C89(H89), C86(H86), C24(H24), C14(H14), C32(H32),
 C41(H41), C15(H15), C28(H28), C29(H29), C44(H44), C16(H16), C48(H48), C36(H36),
  C47(H47), C18(H18), C37(H37), C30(H30), C46(H46), C38(H38), C35(H35),
 C17(H17), C26(H26), C20(H20), C22(H22), C45(H45), C39(H39), C34(H34), C23(H23),
  C6(H6), C27(H27), C40(H40), C3(H3), C33(H33), C5(H5), C21(H21), C4(H4)
5.c Idealised Me refined as rotating group:
 C49(H49a,H49b,H49c), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              1849
_shelx_hkl_checksum              7977
_olex2_submission_special_instructions 'No special instructions were received'