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_1549565
_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         'C48 H44 Cl2 Os P2 Si, C H2 Cl2'
_chemical_formula_sum            'C49 H46 Cl4 Os P2 Si'
_chemical_formula_weight         1056.89
_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             2017-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-12-08 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8290(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.60758(19)
_cell_length_b                   16.9798(3)
_cell_length_c                   22.4892(4)
_cell_measurement_reflns_used    4323
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4990
_cell_measurement_theta_min      3.9440
_cell_volume                     4416.76(13)
_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 0.990
_diffrn_measured_fraction_theta_max 0.988
_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     80.00 178.00   1.00    4.00    --  110.57  30.00 -60.00   98
  2  \w    -70.00  31.00   1.00    2.00    --  -40.57  57.00-120.00  101
  3  \w   -117.00 -14.00   1.00    2.00    --  -40.57 -37.00  30.00  103
  4  \w    100.00 176.00   1.00    4.00    --  110.57 111.00 120.00   76
  5  \w     85.00 178.00   1.00    4.00    --  110.57  45.00-120.00   93
  6  \w     37.00 141.00   1.00    4.00    --  110.57 -61.00  30.00  104
;
_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      -0.0017044000
_diffrn_orient_matrix_UB_12      -0.0019740000
_diffrn_orient_matrix_UB_13      -0.0685599000
_diffrn_orient_matrix_UB_21      -0.0638314000
_diffrn_orient_matrix_UB_22      -0.0796471000
_diffrn_orient_matrix_UB_23      -0.0009698000
_diffrn_orient_matrix_UB_31      -0.1167679000
_diffrn_orient_matrix_UB_32      0.0435387000
_diffrn_orient_matrix_UB_33      -0.0050352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13755
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.266
_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    8.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85386
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.535
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6008
_reflns_number_total             7871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02086h2.cif
_cod_data_source_block           ruan29cult
_cod_depositor_comments
'Adding full bibliography for 1549565--1549567.cif.'
_cod_original_cell_volume        4416.77(13)
_cod_database_code               1549565
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Os Cl2 P2 C42 Si C4 H50'
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.718
_reflns_odcompleteness_completeness 98.62
_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.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), 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)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              97905
_olex2_date_sample_data_collection 2017-07-19
_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.758