Octametallic Cluster of Cp*Ir(glycinato) Cations.
Morris, David M.; Merola, Joseph S.; ACS omega 4 (2019) 22126–22132; doi:10.1021/acsomega.9b03267

data_4517193
_publ_section_title
;
 Octametallic Cluster of Cp*Ir(glycinato) Cations.
;
_journal_issue                   26
_journal_name_full               'ACS omega'
_journal_page_first              22126
_journal_page_last               22132
_journal_paper_doi               10.1021/acsomega.9b03267
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C96 H152 Ir8 N8 O16, 8(F6 P)'
_chemical_formula_sum            'C96 H152 F48 Ir8 N8 O16 P8'
_chemical_formula_weight         4371.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-17
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
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_cell_length_b                   12.7541(3)
_cell_length_c                   36.915(2)
_cell_measurement_reflns_used    33581
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      32.3992
_cell_measurement_theta_min      3.5863
_cell_volume                     14726.3(13)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
  1 omega  -32.00    1.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190  128.0000  -78.0000 33

  2 omega   57.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190  178.0000   60.0000 25

  3 omega    9.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       29.2190 -103.0000  -70.0000 58

  4 omega  -98.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753    0.0000   60.0000 137

  5 omega  -71.00   22.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  103.0000   31.0000 93

  6 omega -100.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000  -90.0000 94

  7 omega  -61.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000  120.0000 65

  8 omega  -57.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000 -180.0000 51

  9 omega  -62.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   77.0000 -150.0000 105

 10 omega  -49.00    0.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -38.0000    0.0000 49

 11 omega  -97.00   -7.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000    0.0000 90

 12 omega  -40.00   41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   57.0000  150.0000 81
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
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_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            148505
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.362
_diffrn_reflns_theta_min         3.604
_exptl_absorpt_coefficient_mu    7.400
_exptl_absorpt_correction_T_max  0.267
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_description       irregular
_exptl_crystal_F_000             8320
_exptl_crystal_preparation       'From Cp*Ir(gly)Cl and AgPF6'
_exptl_crystal_recrystallization_method 'From DCM and Hexanes'
_exptl_crystal_size_max          0.3289
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.2339
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_refine_ls_number_parameters     849
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+342.4212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_depositor_comments
'Adding full bibliography for 4517188--4517193.cif.'
_cod_original_cell_volume        14726.5(13)
_cod_database_code               4517193
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C42(H42A,H42B), C44(H44A,
 H44B), C46(H46A,H46B), C48(H48A,H48B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              18131
_shelx_hkl_checksum              81086
_shelx_fab_checksum              15239
_olex2_submission_special_instructions 'No special instructions were received'