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_4077926
_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         'C36 H30 B1 Cl2 Ir2 Mo2 N6 O10 Si1 W1'
_chemical_formula_sum            'C36 H30 B Cl2 Ir2 Mo2 N6 O10 Si W'
_chemical_formula_weight         1576.64
_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
_audit_creation_date             09-12-16
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 110.0194(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4282(4)
_cell_length_b                   14.7952(3)
_cell_length_c                   17.9635(3)
_cell_measurement_reflns_used    130107
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4352.08(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.141
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            85532
_diffrn_reflns_theta_full        27.473
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.686
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.499
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.324
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.406
_exptl_crystal_density_method    'noe measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.76
_refine_diff_density_min         -3.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9930
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001093
_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: 
 61.7 96.6 48.3 12.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1846
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1846
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                6824
_reflns_number_total             9957
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.13
_oxford_diffrn_Wilson_scale      143.43
_oxford_refine_ls_r_factor_ref   0.0628
_oxford_refine_ls_scale          0.10458(4)
_oxford_reflns_number_all        9930
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '12161130 ran046'
_cod_data_source_file            om201053s_si_001.cif
_cod_data_source_block           ran046
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 21/n 1 '
_cod_original_formula_sum        'C36 H30 B1 Cl2 Ir2 Mo2 N6 O10 Si1 W1'
_cod_database_code               4077926