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_4125902
_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 Li5 O4 Rh Si4'
_chemical_formula_sum            'C40 H80 Li5 O4 Rh Si4'
_chemical_formula_weight         875.01
_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             2016-11-01
_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                 92.763(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0164(8)
_cell_length_b                   20.6077(14)
_cell_length_c                   20.6174(15)
_cell_measurement_reflns_used    5518
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      24.8290
_cell_measurement_theta_min      3.3700
_cell_volume                     5099.6(6)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -19.00   52.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -99.0000  -30.0000 71

  2 omega  -20.00   30.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -99.0000    0.0000 50

  3 omega  -25.00    4.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954    0.0000 -180.0000 29

  4 omega  -79.00  -52.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -19.0000  -90.0000 27

  5 omega  -16.00   11.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -19.0000  -90.0000 27

  6 omega   -7.00   32.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -19.0000  -30.0000 39

  7 omega  -20.00   63.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954   38.0000 -120.0000 83

  8 omega  -87.00    9.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -38.0000   90.0000 96

  9 omega  -16.00   11.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   38.0000  -90.0000 27

 10 omega  -20.00   53.00   1.0000    4.3000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -99.0000  150.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0454998000
_diffrn_orient_matrix_UB_12      -0.0210598000
_diffrn_orient_matrix_UB_13      -0.0074975000
_diffrn_orient_matrix_UB_21      0.0368808000
_diffrn_orient_matrix_UB_22      -0.0268925000
_diffrn_orient_matrix_UB_23      0.0006759000
_diffrn_orient_matrix_UB_31      -0.0079596000
_diffrn_orient_matrix_UB_32      -0.0041614000
_diffrn_orient_matrix_UB_33      0.0336121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31369
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84197
_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    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5684
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0862
_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^)+(0.0499P)^2^+62.1778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1856
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                4475
_reflns_number_total             5684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02039_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        5099.5(6)
_cod_database_code               4125902
_chemical_oxdiff_formula         'C1 O1 Li Rh1 Si1'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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(C14) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C13) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.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), C19(H19A,H19B), C20(H20A,H20B)
3.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'