Spiro Metallaaromatics of Pd, Pt, Rh: Synthesis and Characterization.
Zhang, Yongliang; Wei, Junnian; Chi, Yue; Zhang, Xuan; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b02039

data_4125900
_publ_section_title
;
 Spiro Metallaaromatics of Pd, Pt, Rh: Synthesis and Characterization.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b02039
_journal_year                    2017
_chemical_formula_moiety         'C40 H80 Li4 O4 Pt Si4'
_chemical_formula_sum            'C40 H80 Li4 O4 Pt Si4'
_chemical_formula_weight         960.25
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8849(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8523(2)
_cell_length_b                   20.4652(4)
_cell_length_c                   20.7437(4)
_cell_measurement_reflns_used    19604
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      29.1880
_cell_measurement_theta_min      3.9660
_cell_volume                     5013.31(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  51.00   1.00    5.00    --    9.97 -99.00-120.00   71
  2  \w     34.00  97.00   1.00    5.00    --    9.97-178.00  90.00   63
  3  \w     38.00  76.00   1.00    5.00    --    9.97-178.00-120.00   38
  4  \w    -63.00  24.00   1.00    5.00    --    9.97 -38.00-180.00   87
  5  \w    -19.00  32.00   1.00    5.00    --    9.97 -38.00  30.00   51
  6  \w     26.00  53.00   1.00    5.00    --    9.97  38.00  90.00   27
  7  \w    -13.00  31.00   1.00    5.00    --    9.97  57.00-180.00   44
  8  \w    -62.00   1.00   1.00    5.00    --    9.97 -57.00 -30.00   63
  9  \w     -9.00  29.00   1.00    5.00    --  -11.85 -99.00-120.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0335106000
_diffrn_orient_matrix_UB_12      0.0126602000
_diffrn_orient_matrix_UB_13      -0.0238597000
_diffrn_orient_matrix_UB_21      0.0491432000
_diffrn_orient_matrix_UB_22      -0.0135382000
_diffrn_orient_matrix_UB_23      0.0168114000
_diffrn_orient_matrix_UB_31      -0.0082075000
_diffrn_orient_matrix_UB_32      -0.0292967000
_diffrn_orient_matrix_UB_33      -0.0180505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29543
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4942
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+5.5691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                4802
_reflns_number_total             4942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02039_si_002.cif
_cod_data_source_block           3a
_cod_database_code               4125900
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(H18C)=Sof(H18D)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(H20A)=Sof(H20B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C18(H18C,H18D), C19(H19A,H19B), C19'(H19C,H19D),
 C20(H20A,H20B), C20(H20C,H20D)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_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 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.675