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_4077927
_publ_section_related_literature
; 
? 
;
_publ_section_title
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 Mixed-Metal Cluster Chemistry. 31.(1) Reactions of
 Dimolybdenum--Diiridium Clusters with Alkylidyne Complexes
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_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         'C35 H28 B1 Cl2 Ir2 Mo3 N6 O8'
_chemical_formula_sum            'C35 H28 B Cl2 Ir2 Mo3 N6 O8'
_chemical_formula_weight         1414.62
_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
_audit_creation_date             09-12-22
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                78.7340(16)
_cell_angle_beta                 85.573(2)
_cell_angle_gamma                89.436(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6240(3)
_cell_length_b                   12.8133(5)
_cell_length_c                   13.7322(5)
_cell_measurement_reflns_used    47284
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     1999.87(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.090
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41718
_diffrn_reflns_theta_full        26.999
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.584
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.737
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.01
_refine_diff_density_min         -2.14
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8722
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000450
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 14.9 21.8 11.3 3.23 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1423
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1423
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5930
_reflns_number_total             9201
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0685
_oxford_refine_ls_scale          0.09635(3)
_oxford_reflns_number_all        9175
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '6241041 ran023'
_cod_data_source_file            om201053s_si_001.cif
_cod_data_source_block           ran023
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C35 H28 B1 Cl2 Ir2 Mo3 N6 O8'
_cod_database_code               4077927