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_4517190
_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_absolute_configuration ad
_chemical_formula_moiety         'C14 H22 Ir N2 O2, B F4'
_chemical_formula_sum            'C14 H22 B F4 Ir N2 O2'
_chemical_formula_weight         529.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-11-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.931(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7519(2)
_cell_length_b                   8.57120(10)
_cell_length_c                   11.3815(2)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    99.8(5)
_cell_measurement_theta_max      31.7190
_cell_measurement_theta_min      3.9930
_cell_volume                     914.79(3)
_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)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -35.00   -8.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   90.0000 27

  2 omega  -24.00    7.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -84.0000   59.3229 31

  3 omega  -25.00    6.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -82.0000  -69.2257 31

  4 omega  -50.00   38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   38.0000   60.0000 88

  5 omega  -45.00   -7.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -120.0000 38

  6 omega  -24.00    4.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -81.0000 -167.4227 28

  7 omega  -94.00   -7.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000    0.0000 87

  8 omega  -92.00  -60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000 -120.0000 32

  9 omega -102.00  -20.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -38.0000  -90.0000 82

 10 omega  -56.00   43.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000 -150.0000 99

 11 omega  -62.00   27.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000  -60.0000 89

 12 omega -100.00  -49.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000   90.0000 51

 13 omega  -99.00  -10.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -57.0000  150.0000 89

 14 omega  -68.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000   60.0000 33

 15 omega -103.00  -36.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000    0.0000 67

 16 omega  -98.00  -43.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  141.0000  -10.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_UB_11      -0.0301025000
_diffrn_orient_matrix_UB_12      -0.0019795000
_diffrn_orient_matrix_UB_13      0.0500679000
_diffrn_orient_matrix_UB_21      -0.0690708000
_diffrn_orient_matrix_UB_22      -0.0072579000
_diffrn_orient_matrix_UB_23      -0.0410524000
_diffrn_orient_matrix_UB_31      0.0067978000
_diffrn_orient_matrix_UB_32      -0.0824180000
_diffrn_orient_matrix_UB_33      0.0024246000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.423
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.344
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.140
_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    1.922
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_preparation       'From Cp*Ir(glycine)Cl and AgBF4 in H3CN'
_exptl_crystal_size_max          0.5888
_exptl_crystal_size_mid          0.2064
_exptl_crystal_size_min          0.1389
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.286(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         6111
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                5549
_reflns_number_total             6111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03267_si_002.cif
_cod_data_source_block           dmmxi063a_abs_compound_3
_cod_depositor_comments
'Adding full bibliography for 4517188--4517193.cif.'
_cod_database_code               4517190
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C12 H18 B  F4 Ir N O2'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.714(12)
 0.286(12)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C12(H12A,H12B)
3.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), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              78994
_shelx_hkl_checksum              16547
_olex2_exptl_crystal_mounting_method fiber
_olex2_submission_original_sample_id DMMXI063a
_olex2_submission_special_instructions 'No special instructions were received'