Halogenation of carbyne complexes: isolation of unsaturated metallaiodirenium ion and metallabromirenium ion
Luo, Ming; Zhu, Congqing; Chen, Lina; Zhang, Hong; Xia, Haiping; Chem. Sci. 7 (2016) 1815–; doi:10.1039/C5SC03963K

data_1540560
_publ_section_title
;
 Halogenation of carbyne complexes: isolation of unsaturated
 metallaiodirenium ion and metallabromirenium ion
;
_journal_issue                   3
_journal_name_full               'Chem. Sci.'
_journal_page_first              1815
_journal_paper_doi               10.1039/C5SC03963K
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety
'C63 H51 Cl I O2 Os P3, 2(Cl2 I), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C64.5 H54 Cl8 I3 O2 Os P3'
_chemical_formula_weight         1808.48
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-27 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.771(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9311(5)
_cell_length_b                   22.2426(7)
_cell_length_c                   23.2785(8)
_cell_measurement_reflns_used    9095
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.4020
_cell_measurement_theta_min      3.1710
_cell_volume                     6529.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27557
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.962
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55209
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3492
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.549
_refine_diff_density_min         -1.388
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         11489
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0439P)^2^+43.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9876
_reflns_number_total             11489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03963k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1540560--1540561.cif.'
_cod_original_formula_sum        'C64.50 H54 Cl8 I3 O2 Os P3'
_cod_database_code               1540560
_shelxl_version_number           2013-4
_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. Shared sites
{C131, C2D}
3. Restrained distances
 Cl3-I2
 2.55 with sigma of 0.02
 Cl2D-C1D
 1.77 with sigma of 0.02
 Cl2-I2
 2.55 with sigma of 0.02
 Cl1D-C1D
 1.77 with sigma of 0.02
 Cl2D-Cl1D
 2.79 with sigma of 0.02
 Cl6D-Cl3D
 2.79 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl6D) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl5D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl5D) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2D) \\sim Ueq, Uanis(C131) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(Cl6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C131) = Uanis(C2D)
5. Others
 Fixed Sof: I2(0.25) I4(0.25) Cl7(0.25) Cl3(0.25) Cl6(0.25) Cl2(0.25)
 Cl4D(0.5) Cl3D(0.5) Cl6D(0.5) Cl1D(0.5) Cl2D(0.5) C131(0.5) H13a(0.5)
 H13b(0.5) C2D(0.5) H2Da(0.5) H2Db(0.5) C1D(0.5) H1Da(0.5) H1Db(0.5) Cl5D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C131(H13a,H13b), C2D(H2Da,H2Db), C1D(H1Da,H1Db)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C40P(H40P), C20P(H20P), C51P(H51P), C14P(H14P), C54P(H54P),
 C22P(H22P), C12P(H12P), C27P(H27P), C5P(H5P), C42P(H42P), C38P(H38P), C2P(H2P),
  C30P(H30P), C3(H3), C53P(H53P), C6P(H6P), C3P(H3P), C5AA(H5AA), C18P(H18P),
 C34P(H34P), C52P(H52P), C50P(H50P), C28P(H28P), C21P(H21P), C9P(H9P),
 C32P(H32P), C23P(H23P), C26P(H26P), C41P(H41P), C8P(H8P), C11P(H11P),
 C24P(H24P), C35P(H35P), C29P(H29P), C17P(H17P), C39P(H39P), C33P(H33P),
 C4P(H4P), C15P(H15P), C16P(H16P), C5(H5), C48P(H48P), C45P(H45P), C47P(H47P),
 C10P(H10P), C44P(H44P), C46P(H46P)
6.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c)
;
_shelx_res_checksum              60049
_olex2_submission_special_instructions 'No special instructions were received'