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_4517192
_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
'C36 H57 Ir3 N3 O6, 3(B F4), 5(C3 H7 N O), C3 H6'
_chemical_formula_sum            'C54 H98 B3 F12 Ir3 N8 O11'
_chemical_formula_weight         1872.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                97.538(2)
_cell_angle_beta                 93.547(2)
_cell_angle_gamma                94.776(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8589(3)
_cell_length_b                   12.0553(3)
_cell_length_c                   24.3256(6)
_cell_measurement_reflns_used    23616
_cell_measurement_temperature    100.05(10)
_cell_measurement_theta_max      32.1160
_cell_measurement_theta_min      3.8050
_cell_volume                     3426.29(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
  1 omega  -21.00   38.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   57.0000  -60.0000 59

  2 omega  -60.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000    0.0000 102

  3 omega  -62.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000 -180.0000 104

  4 omega  -31.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000 -150.0000 35

  5 omega  -79.00  -51.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -77.0000 -150.0000 28

  6 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -120.0000 94

  7 omega  -20.00    5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -85.0000   32.1059 25

  8 omega  -23.00    5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -82.0000  111.3713 28

  9 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  150.0000 94

 10 omega  -62.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000   90.0000 105

 11 omega  -71.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   95.0000 -123.0000 99

 12 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   60.0000 94

 13 omega -100.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  -30.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            78945
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.503
_diffrn_reflns_theta_min         3.581
_exptl_absorpt_coefficient_mu    5.903
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.815
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_preparation       'Cp*Ir(glycine)Cl and AgBF4'
_exptl_crystal_recrystallization_method 'From DMF and hexanes'
_exptl_crystal_size_max          0.4193
_exptl_crystal_size_mid          0.1983
_exptl_crystal_size_min          0.1181
_refine_diff_density_max         2.213
_refine_diff_density_min         -2.219
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         22990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+8.8381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18886
_reflns_number_total             22990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03267_si_002.cif
_cod_data_source_block           dmmxi062a_abs_compound_5
_cod_depositor_comments
'Adding full bibliography for 4517188--4517193.cif.'
_cod_database_code               4517192
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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), C32(H32A,H32B), C34(H34A,H34B),
 C36(H36A,H36B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
2.b Aromatic/amide H refined with riding coordinates:
 C13D(H13D), C4D(H4D), C7D(H7D), C12D(H12D), C2AA(H2AA)
2.c 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),
 C14D(H14A,H14B,H14C), C15D(H15A,H15B,H15C), C5D(H5DA,H5DB,H5DC), C6D(H6DA,H6DB,
 H6DC), C8D(H8DA,H8DB,H8DC), C9D(H9DA,H9DB,H9DC), C10D(H10D,H10E,H10F),
 C11D(H11A,H11B,H11C), C3AA(H3AA,H3AB,H3AC), C4AA(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              13931
_shelx_hkl_checksum              64193
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_special_instructions 'No special instructions were received'