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_4125899
_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 H72 Li4 O4 Pd'
_chemical_formula_sum            'C40 H72 Li4 O4 Pd'
_chemical_formula_weight         751.14
_chemical_name_systematic        4EtPd
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.426(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1080(8)
_cell_length_b                   10.0450(5)
_cell_length_c                   23.5630(9)
_cell_measurement_reflns_used    7558
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      29.0560
_cell_measurement_theta_min      3.5920
_cell_volume                     4359.7(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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      180.01(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   -4.00   77.00   1.0000    4.4400
omega____ theta____ kappa____ phi______ frames
    -       10.7017   77.0000   90.0000 81

  2 omega   38.00   87.00   1.0000    4.4400
omega____ theta____ kappa____ phi______ frames
    -       10.7017   38.0000 -150.0000 49

  3 omega  -99.00  -70.00   1.0000    4.4400
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  178.0000  120.0000 29

  4 omega  -20.00   16.00   1.0000    4.4400
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -99.0000    0.0000 36

  5 omega  -25.00    8.00   1.0000    4.4400
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -77.0000  -60.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0195627000
_diffrn_orient_matrix_UB_12      0.0186983000
_diffrn_orient_matrix_UB_13      -0.0204598000
_diffrn_orient_matrix_UB_21      0.0186694000
_diffrn_orient_matrix_UB_22      -0.0617117000
_diffrn_orient_matrix_UB_23      0.0045715000
_diffrn_orient_matrix_UB_31      -0.0274182000
_diffrn_orient_matrix_UB_32      -0.0286951000
_diffrn_orient_matrix_UB_33      -0.0231636000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22698
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85232
_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 black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         8579
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+4.9024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                6487
_reflns_number_total             8579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02039_si_002.cif
_cod_data_source_block           2c
_cod_database_code               4125899
_chemical_oxdiff_formula         'C1 H1 Pd1 O1'
_reflns_odcompleteness_completeness 99.71
_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
O1 \\sim C18: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C34) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C17) \\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), C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B),
 C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), 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)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,
 H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'