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_1549566
_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, C H2 Cl2'
_chemical_formula_sum            'C53 H48 Cl4 Os P2 Si'
_chemical_formula_weight         1106.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9889(2)
_cell_length_b                   16.4530(2)
_cell_length_c                   21.3301(3)
_cell_measurement_reflns_used    5661
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.8200
_cell_measurement_theta_min      4.0000
_cell_volume                     4869.82(11)
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_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     39.00 137.00   1.00    2.00    --  110.57 -30.00  60.00   98
  2  \w    -70.00  30.00   1.00    1.00    --  -40.57  57.00 -30.00  100
  3  \w   -117.00 -15.00   1.00    1.00    --  -40.57 -37.00  30.00  102
  4  \w     38.00 133.00   1.00    2.00    --  110.57 -77.00  60.00   95
  5  \w     33.00 115.00   1.00    2.00    --  110.57-111.00-120.00   82
  6  \w     64.00 151.00   1.00    2.00    --  110.57 178.00 120.00   87
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1047573000
_diffrn_orient_matrix_UB_12      0.0253715000
_diffrn_orient_matrix_UB_13      -0.0226777000
_diffrn_orient_matrix_UB_21      -0.0136327000
_diffrn_orient_matrix_UB_22      -0.0768893000
_diffrn_orient_matrix_UB_23      -0.0413317000
_diffrn_orient_matrix_UB_31      -0.0343262000
_diffrn_orient_matrix_UB_32      -0.0470896000
_diffrn_orient_matrix_UB_33      0.0554257000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7646
_diffrn_reflns_point_group_measured_fraction_full 0.627
_diffrn_reflns_point_group_measured_fraction_max 0.624
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.488
_diffrn_reflns_theta_min         3.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86039
_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            brown
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.475
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         5484
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.219
_reflns_Friedel_fraction_full    0.238
_reflns_Friedel_fraction_max     0.233
_reflns_number_gt                5361
_reflns_number_total             5484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02086h2.cif
_cod_data_source_block           ruan31cult
_cod_depositor_comments
'Adding full bibliography for 1549565--1549567.cif.'
_cod_database_code               1549566
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 Cl1S-C1S \\sim Cl2S-C1S
 with sigma of 0.02
 Cl1A-C1SA \\sim Cl2A-C1SA
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) Cl1S(0.5) Cl2S(0.5) C1SA(0.5)
 H1SC(0.5) H1SD(0.5) Cl1A(0.5) Cl2A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C1SA(H1SC,H1SD)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52),
 C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65),
  C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              81430
_olex2_date_sample_data_collection 2017-08-25
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.841