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_7036669
_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_sum            'C40 H74 Ir4 N21 O40 P W12'
_chemical_formula_weight         4495.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-06 deposited with the CCDC.
2015-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.138(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7020(3)
_cell_length_b                   36.5532(8)
_cell_length_c                   22.0062(15)
_cell_measurement_reflns_used    30796
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.2
_cell_measurement_theta_min      2.0
_cell_volume                     9359.1(7)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device
;
AFC11 (Left): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn944+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1901
_diffrn_reflns_av_sigmaI/netI    0.1158
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            223893
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    37.975
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             7968
_exptl_crystal_recrystallization_method 'Counterdiffusion in agarose gel'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 80 water molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions
by SQUEEZE/PLATON. These solvent molecules are allocated in monodimensional 
channels (voids) along the [1 0 0] direction, occupying around 20% of the 
volume of the unit cell (ca. 2000 A3).
;
_refine_diff_density_max         5.198
_refine_diff_density_min         -4.993
_refine_diff_density_rms         0.425
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1032
_refine_ls_number_reflns         16296
_refine_ls_number_restraints     704
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3096
_refine_ls_wR_factor_ref         0.3353
_reflns_number_gt                10011
_reflns_number_total             16296
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03302k2.cif
_cod_data_source_block           gel
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036668--7036669.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7036669