Facile synthesis of polycyclic metallaarynes.
Ruan, Wenqing; Leung, Tsz-Fai; Shi, Chuan; Lee, Ka Ho; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Chemical science 9 (2018) 5994–5998; doi:10.1039/c8sc02086h

data_1549567
_publ_section_title
;
 Facile synthesis of polycyclic metallaarynes.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              5994
_journal_page_last               5998
_journal_paper_doi               10.1039/c8sc02086h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C52 H46 Cl2 Os P2 Si, 3(C H2 Cl2)'
_chemical_formula_sum            'C55 H52 Cl8 Os P2 Si'
_chemical_formula_weight         1276.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2018-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8377(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4227(2)
_cell_length_b                   17.2735(3)
_cell_length_c                   13.9125(3)
_cell_measurement_reflns_used    8846
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.3830
_cell_measurement_theta_min      4.1460
_cell_volume                     2676.46(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     34.00 137.00   1.00   20.00    --  110.57 -77.00 150.00  103
  2  \w    -69.00  33.00   1.00    5.00    --  -40.20  77.00   0.00  102
  3  \w      1.00  50.00   1.00    5.00    --   40.20 -99.00 120.00   49
  4  \w   -115.00 -14.00   1.00    5.00    --  -40.20 -37.00-120.00  101
  5  \w   -112.00 -11.00   1.00    5.00    --  -40.20 -57.00 150.00  101
  6  \w     56.00  82.00   1.00    5.00    --   40.20 -99.00 120.00   26
  7  \w     49.00 142.00   1.00   20.00    --  110.57 -77.00 -30.00   93
  8  \w     83.00 176.00   1.00   20.00    --  110.57  45.00  90.00   93
  9  \w     57.00 151.00   1.00   20.00    --  110.57 178.00-120.00   94
 10  \w     37.00 140.00   1.00   20.00    --  110.57 -30.00 120.00  103
 11  \w     35.00 115.00   1.00   20.00    --  110.57-111.00 -30.00   80
 12  \w     40.00 141.00   1.00   20.00    --  110.57 -30.00 -90.00  101
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15170
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.969
_exptl_absorpt_coefficient_mu    9.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         4986
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+10.4102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4638
_reflns_number_total             4986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02086h2.cif
_cod_data_source_block           ruan35a
_cod_depositor_comments
'Adding full bibliography for 1549565--1549567.cif.'
_cod_database_code               1549567
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.404
_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
 Cl3S-C2S = Cl4S-C2S
 1.72 with sigma of 0.02
 C32A-C31A \\sim C33A-C32A \\sim C34A-C33A \\sim C34A-C35A \\sim C36A-C35A
\\sim C36A-C31A
 with sigma of 0.02
 C32-C31 \\sim C33-C32 \\sim C34-C33 \\sim C34-C35 \\sim C36-C35 \\sim C36-C31
 with sigma of 0.02
 Si1-C15 \\sim Si1-C14 \\sim Si1-C16
 with sigma of 0.02
 Cl3S-C2S \\sim Cl4S-C2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Si1(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C31(0.5) C31A(0.5)
 C32(0.5) H32(0.5) C32A(0.5) H32A(0.5) C33(0.5) H33(0.5) C33A(0.5) H33A(0.5)
 C34(0.5) H34(0.5) C34A(0.5) H34A(0.5) C35(0.5) H35(0.5) C35A(0.5) H35A(0.5)
 C36(0.5) H36(0.5) C36A(0.5) H36A(0.5) Cl3S(0.5) Cl4S(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C32A(H32A), C33(H33),
 C33A(H33A), C34(H34), C34A(H34A), C35(H35), C35A(H35A), C36(H36), C36A(H36A),
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;