Gel-assisted crystallization of [Ir4(IMe)7(CO)H10](2+) and [Ir4(IMe)8H9](3+) clusters derived from catalytic glycerol dehydrogenation.
Sharninghausen, Liam S.; Mercado, Brandon Q.; Crabtree, Robert H.; Balcells, David; Campos, Jesús; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18403–18410; doi:10.1039/c5dt03302k

data_7036668
_publ_section_title
;
 Gel-assisted crystallization of [Ir4(IMe)7(CO)H10](2+) and
 [Ir4(IMe)8H9](3+) clusters derived from catalytic glycerol
 dehydrogenation.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18403
_journal_page_last               18410
_journal_paper_doi               10.1039/c5dt03302k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'2(C32 H12 B F24), C36 H56 Ir4 N14, 1.5(C6H6)'
_chemical_formula_sum            'C109 H89 B2 F48 Ir4 N14 O'
_chemical_formula_weight         3313.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-07-06 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                91.664(7)
_cell_angle_beta                 107.958(8)
_cell_angle_gamma                106.800(7)
_cell_formula_units_Z            2
_cell_length_a                   14.6752(3)
_cell_length_b                   20.0841(5)
_cell_length_c                   22.7318(16)
_cell_measurement_reflns_used    78689
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6049.9(6)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            107549
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    4.512
_exptl_absorpt_correction_T_max  0.571
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3198
_exptl_crystal_recrystallization_method 'Diffusion in gel matrix'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.520
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1887
_refine_ls_number_reflns         27634
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+26.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20206
_reflns_number_total             27634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03302k2.cif
_cod_data_source_block           spider-14151
_cod_depositor_comments
'Adding full bibliography for 7036668--7036669.cif.'
_cod_database_code               7036668
_shelx_estimated_absorpt_t_min   0.497
_shelx_estimated_absorpt_t_max   0.571
_shelxl_version_number           2014/6
_shelx_res_checksum              93157
_shelx_fab_checksum              50065