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_4517189
_publ_section_title
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 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         'C12 H19 Cl Ir N O2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C12.5 H20 Cl2 Ir N O2'
_chemical_formula_weight         479.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-11-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8063(3)
_cell_length_b                   14.5872(3)
_cell_length_c                   16.3284(3)
_cell_measurement_reflns_used    6320
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      32.2761
_cell_measurement_theta_min      3.6849
_cell_volume                     3050.28(11)
_computing_cell_refinement
;
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
;
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
;
CrysAlisPro, Oxford Diffraction Ltd.,

Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)

(compiled Oct 25 2010,18:11:34)
;
_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-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.1
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;

  1 omega  -97.00  -31.00   1.0000   16.0000

omega____ theta____ kappa____ phi______ frames

    -      -29.3753  -77.0000   60.0000 66

  2 omega  -77.00  -35.00   1.0000   16.0000

omega____ theta____ kappa____ phi______ frames

    -      -29.3753 -178.0000   30.0000 42

  3 omega -107.00  -54.00   1.0000   16.0000

omega____ theta____ kappa____ phi______ frames

    -      -29.3753 -178.0000  -90.0000 53
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0321471000
_diffrn_orient_matrix_UB_12      0.0336532000
_diffrn_orient_matrix_UB_13      0.0184368000
_diffrn_orient_matrix_UB_21      0.0430221000
_diffrn_orient_matrix_UB_22      -0.0152902000
_diffrn_orient_matrix_UB_23      -0.0238087000
_diffrn_orient_matrix_UB_31      -0.0136439000
_diffrn_orient_matrix_UB_32      0.0315406000
_diffrn_orient_matrix_UB_33      -0.0313230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11594
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.349
_diffrn_reflns_theta_min         3.692
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.100
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
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    2.088
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_preparation       'From [Cp*IrCl2]2 and L-glycine with base'
_exptl_crystal_recrystallization_method 'From DCM'
_exptl_crystal_size_max          0.2383
_exptl_crystal_size_mid          0.1713
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details
;
 Flack x determined using 2693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8796
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.594
_reflns_Friedel_fraction_full    0.777
_reflns_Friedel_fraction_max     0.669
_reflns_number_gt                7930
_reflns_number_total             8796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03267_si_002.cif
_cod_data_source_block           dmmxi029a_abs_compound_2
_cod_depositor_comments
;
Adding full bibliography for 4517188--4517193.cif.

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C25 H40 Cl4 Ir2 N2 O4'
_cod_original_formula_weight         958.79
_cod_original_formula_moiety         '2(C12 H19 Cl Ir N O2), C H2 Cl2'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        3050.27(10)
_cod_database_code               4517189
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C25 H40 Cl4 Ir2 N2 O4'
_chemical_oxdiff_usercomment     dmmxI029a
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.220
_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. Restrained distances
 N2-H2A = N2-H2B = N1-H1A = N1-H1B
 1 with sigma of 0.05
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), N1(H1A,H1B), C24(H24A,H24B), C25(H25A,H25B)
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), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              68500
_shelx_hkl_checksum              30437
_olex2_exptl_crystal_mounting_method 'On fiber'
_olex2_submission_original_sample_id DMMXI029a
_olex2_submission_special_instructions 'No special instructions were received'