Mixed-Metal Cluster Chemistry. 31.(1) Reactions of Dimolybdenum–Diiridium Clusters with Alkylidyne Complexes
Randles, Michael D.; Dewhurst, Rian D.; Cifuentes, Marie P.; Humphrey, Mark G.; Organometallics 31 (2012) 2582–; doi:10.1021/om201053s

data_4077925
_publ_section_title
;
 Mixed-Metal Cluster Chemistry. 31.(1) Reactions of
 Dimolybdenum--Diiridium Clusters with Alkylidyne Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2582
_journal_paper_doi               10.1021/om201053s
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        local
_chemical_formula_moiety         'C43 H42 B Ir2 Mo3 N6 O9, 2(C H Cl3)'
_chemical_formula_sum            'C45 H44 B Cl6 Ir2 Mo3 N6 O9'
_chemical_formula_weight         1708.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                81.7881(6)
_cell_angle_beta                 88.8624(7)
_cell_angle_gamma                78.6851(5)
_cell_formula_units_Z            4
_cell_length_a                   14.1283(2)
_cell_length_b                   17.1504(2)
_cell_length_c                   23.2541(3)
_cell_measurement_reflns_used    228923
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     5468.25(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            135159
_diffrn_reflns_theta_full        30.059
_diffrn_reflns_theta_max         30.059
_diffrn_reflns_theta_min         2.597
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.869
_exptl_absorpt_correction_T_max  0.342
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.230
_refine_diff_density_max         3.21
_refine_diff_density_min         -2.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9896
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1274
_refine_ls_number_reflns         31865
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.0042624
_refine_ls_shift/su_mean         0.9060516
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +29.93P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1138
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1138
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              24
_reflns_limit_k_min              -23
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                24602
_reflns_number_total             31923
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      117.08
_oxford_refine_ls_r_factor_ref   0.0638
_oxford_refine_ls_scale          0.17625(4)
_oxford_reflns_number_all        31865
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om201053s_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C90 H88 B2 Cl12 Ir4 Mo6 N12 O18'
_cod_original_formula_weight         3417.33
_cod_original_formula_moiety         'C90 H88 B2 Cl12 Ir4 Mo6 N12 O18'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4077925