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_4125901
_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         'C44 H84 Li4 O4 Pt Si4'
_chemical_formula_sum            'C44 H84 Li4 O4 Pt Si4'
_chemical_formula_weight         1012.32
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.039(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0308(4)
_cell_length_b                   22.3313(8)
_cell_length_c                   19.4728(7)
_cell_measurement_reflns_used    25554
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.9800
_cell_measurement_theta_min      2.9250
_cell_volume                     5202.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -21.00   20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191    0.0000 -180.0000 41

  2 omega  -70.00  -39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191    0.0000 -180.0000 31

  3 omega   38.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191 -178.0000   90.0000 63

  4 omega  -11.00   58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   19.0000 -120.0000 69

  5 omega   -7.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000  -60.0000 97

  6 omega  -15.00   22.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191 -103.0000  119.0340 37

  7 omega   -5.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191  -57.0000   90.0000 40

  8 omega   -4.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7128  -99.0000   90.0000 30

  9 omega  -11.00   22.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7128  -99.0000    0.0000 33

 10 omega  -34.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7128   84.0000  -76.0000 26

 11 omega  -13.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6191   38.0000   60.0000 46

 12 omega  -77.00  -29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.7128  133.0000  158.1138 48
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0197192000
_diffrn_orient_matrix_UB_12      -0.0202761000
_diffrn_orient_matrix_UB_13      -0.0265858000
_diffrn_orient_matrix_UB_21      0.0456783000
_diffrn_orient_matrix_UB_22      -0.0193327000
_diffrn_orient_matrix_UB_23      0.0099118000
_diffrn_orient_matrix_UB_31      -0.0322567000
_diffrn_orient_matrix_UB_32      -0.0149685000
_diffrn_orient_matrix_UB_33      0.0231583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65019
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         10238
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0225P)^2^+4.0869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                8593
_reflns_number_total             10238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02039_si_002.cif
_cod_data_source_block           3b
_cod_database_code               4125901
_chemical_oxdiff_formula         'C1 H1 Pt1 Si1 Li1 O1'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
3.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'