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_4517191
_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         '0.67(C45 H69 Ir3 N3 O6), 2(F6 P)'
_chemical_formula_sum            'C30 H46 F12 Ir2 N2 O4 P2'
_chemical_formula_weight         1173.03
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.7694(4)
_cell_length_b                   17.7694(4)
_cell_length_c                   12.1058(3)
_cell_measurement_reflns_used    27940
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.3604
_cell_measurement_theta_min      3.6098
_cell_volume                     3310.32(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  Gemini
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75433
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.434
_diffrn_reflns_theta_min         3.617
_exptl_absorpt_coefficient_mu    6.179
_exptl_absorpt_correction_T_max  0.26
_exptl_absorpt_correction_T_min  0.06
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'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    1.765
_exptl_crystal_description       prism
_exptl_crystal_F_000             1692
_exptl_crystal_preparation       'From Cp*Ir(L-Proline)Cl and AgPF6'
_exptl_crystal_recrystallization_method 'From CH2Cl2 and hexane'
_exptl_crystal_size_max          0.4389
_exptl_crystal_size_mid          0.2301
_exptl_crystal_size_min          0.1865
_refine_diff_density_max         5.202
_refine_diff_density_min         -1.916
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 2394 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         7678
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.482
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+26.1354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                5668
_reflns_number_total             7678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03267_si_002.cif
_cod_data_source_block           dmmxi018a_abs_cp_compound_4
_cod_depositor_comments
'Adding full bibliography for 4517188--4517193.cif.'
_cod_original_cell_volume        3310.32(17)
_cod_database_code               4517191
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C1A, C1B, C2A, C2B, C3A, C3B, C4A, C4B, C5A, C5B, C6A, C6B, C7A, C7B, C8A,
 C8B, C9A, C9B, C10A, C10B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(1)
4.a :
 C1A(C2A,C3A,C4A,C5A,C6A,C7A,C8A,C9A,C10A), C1B(C2B,C3B,C4B,C5B,C6B,C7B,C8B,
 C9B,C10B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), C14(H14)
4.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
4.d Me refined with riding coordinates:
 C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10A,H10B,H10C), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
;
_shelx_res_checksum              41053
_shelx_hkl_checksum              65811
_shelx_fab_checksum              65795
_olex2_exptl_crystal_mounting_method 'On Fiber'
_olex2_submission_original_sample_id DMMXI018a
_olex2_submission_special_instructions 'No special instructions were received'