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_1540561
_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 Br2 O2 Os P3, 2(Br3), C H2 Cl2'
_chemical_formula_sum            'C64 H53 Br8 Cl2 O2 Os P3'
_chemical_formula_weight         1847.35
_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     heavy
_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                 102.857(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0217(3)
_cell_length_b                   22.2992(5)
_cell_length_c                   23.1406(5)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.9618
_cell_measurement_theta_min      2.8020
_cell_volume                     6551.0(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.973
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28371
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.808
_exptl_absorpt_coefficient_mu    7.023
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dull reddish red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.077
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         11541
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0651P)^2^+79.1289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8788
_reflns_number_total             11541
_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_database_code               1540561
_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
{C1D, C3D}
{Cl1D, Cl6D}
3. Restrained distances
 Cl5D-Cl6D
 2.79 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cl3D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl4D) \\sim Ueq, Uanis(C2D) \\sim Ueq, Uanis(Cl2D) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1D) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C1D) = Uanis(C3D)
Uanis(Cl1D) = Uanis(Cl6D)
5. Others
 Fixed Sof: Cl1D(0.5) Cl6D(0.25) Br2B(0.25) Br2A(0.25) Br4A(0.25) Br4B(0.25)
 Cl2D(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) C3D(0.25) H3DA(0.25) H3DB(0.25)
 Br2C(0.25) Cl3D(0.25) Cl4D(0.25) C2D(0.25) H2DA(0.25) H2DB(0.25) Br5(0.125)
 Br6(0.125) Cl5D(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C1D(H1DA,H1DB), C3D(H3DA,H3DB), C2D(H2DA,H2DB)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
6.c Aromatic/amide H refined with riding coordinates:
 C50P(H50P), C3(H3), C36P(H36P), C1(H1), C20P(H20P), C54P(H54P), C5(H5),
 C30P(H30P), C44P(H44P), C48P(H48P), C46P(H46P), C6P(H6P), C15P(H15P),
 C42P(H42P), C45P(H45P), C47P(H47P), C53P(H53P), C46(H46), C41P(H41P),
 C40P(H40P), C28P(H28P), C14P(H14P), C34P(H34P), C21P(H21P), C11P(H11P),
 C35P(H35P), C29P(H29P), C12P(H12P), C3P(H3P), C51P(H51P), C18P(H18P), C2P(H2P),
  C32P(H32P), C16P(H16P), C52P(H52P), C9P(H9P), C38P(H38P), C33P(H33P),
 C24P(H24P), C39P(H39P), C22P(H22P), C10P(H10P), C17P(H17P), C26P(H26P),
 C27P(H27P), C23P(H23P), C5P(H5P), C4P(H4P)
;
_shelx_res_checksum              55577
_olex2_submission_special_instructions 'No special instructions were received'