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

data_7132039
_publ_section_title
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 Fused Metallacyclopropenes from Alkynylphenols
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03084A
_journal_year                    2023
_chemical_formula_moiety         'C50 H46 Cl2 O Os P2'
_chemical_formula_sum            'C50 H46 Cl2 O Os P2'
_chemical_formula_weight         985.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.332(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4318(6)
_cell_length_b                   10.3039(2)
_cell_length_c                   22.3306(6)
_cell_measurement_reflns_used    20279
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.9120
_cell_measurement_theta_min      2.1980
_cell_volume                     4219.0(2)
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.200
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66240
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       needle
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.582
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7456
_refine_ls_number_restraints     1128
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0220P)^2^+11.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6341
_reflns_number_total             7456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03084a2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7132039
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.640
_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. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C8 \\sim C7 \\sim C6 \\sim C5: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.001 within 2A
C45 \\sim C39 \\sim C40 \\sim C3 \\sim C27 \\sim C33 \\sim C21 \\sim C44 \\sim
C15 \\sim C50 \\sim C2 \\sim C41 \\sim C26 \\sim C28 \\sim C43 \\sim C47 \\sim
C4 \\sim C49 \\sim C32 \\sim C20 \\sim C34 \\sim C38 \\sim C48 \\sim C22 \\sim
C8 \\sim C16 \\sim C17 \\sim C42 \\sim C46 \\sim C5 \\sim C18 \\sim C23 \\sim
C29 \\sim C19 \\sim C6 \\sim C1 \\sim C31 \\sim C37 \\sim C7 \\sim C25 \\sim
C35 \\sim C12 \\sim C30 \\sim C36 \\sim C24 \\sim C9 \\sim C10 \\sim C14 \\sim
C11 \\sim C13: within 3.8A with sigma of 0.007 and sigma for terminal atoms of
0.014 within 3.8A
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
3. Rigid body (RIGU) restrains
 C7, C6, C5, C4, C3, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C44(H44), C50(H50), C41(H41), C26(H26), C28(H28), C43(H43),
 C47(H47), C49(H49), C32(H32), C20(H20), C34(H34), C38(H38), C48(H48), C22(H22),
  C8(H8), C16(H16), C17(H17), C42(H42), C46(H46), C5(H5), C18(H18), C23(H23),
 C29(H29), C19(H19), C6(H6), C31(H31), C37(H37), C7(H7), C25(H25), C35(H35),
 C30(H30), C36(H36), C24(H24), C9(H9)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              10946
_shelx_hkl_checksum              81967
_olex2_submission_special_instructions 'No special instructions were received'