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

data_7132038
_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_absolute_configuration unk
_chemical_formula_moiety         'C48 H42 Cl2 O Os P2, C H2 Cl2'
_chemical_formula_sum            'C49 H44 Cl4 O Os P2'
_chemical_formula_weight         1042.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-28 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9207(2)
_cell_length_b                   12.9359(2)
_cell_length_c                   30.7710(6)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.53
_cell_volume                     4346.99(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       '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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            45361
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         2.441
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.290
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0845 before and 0.0738 after correction.
The Ratio of minimum to maximum transmission is 0.3877.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic brownish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 3484 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0161P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0458
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                8303
_reflns_number_total             8846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03084a2.cif
_cod_data_source_block           1
_cod_database_code               7132038
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.439
_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:
 C11(H11A,H11B), C10(H10A,H10B), C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C39(H39), C40(H40), C32(H32), C5(H5), C8(H8), C26(H26),
 C36(H36), C46(H46), C48(H48), C30(H30), C41(H41), C47(H47), C38(H38), C45(H45),
  C33(H33), C44(H44), C29(H29), C18(H18), C14(H14), C27(H27), C15(H15),
 C28(H28), C9(H9), C22(H22), C24(H24), C16(H16), C42(H42), C34(H34), C17(H17),
 C23(H23), C20(H20), C35(H35), C21(H21)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              17799
_shelx_hkl_checksum              31264
_olex2_submission_special_instructions 'No special instructions were received'