Bis(diphosphino)methanide and hydride derivatives of Ir4(CO)12
Detti, Serena; Lumini, Tito; Roulet, Raymond; Schenk, Kurt; Ros, Renzo; Tassan, Augusto; Journal of the Chemical Society, Dalton Transactions  (2000) 1645–; doi:10.1039/a909881j

data_7009303
_publ_section_title
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 Bis(diphosphino)methanide and hydride derivatives of Ir4(CO)12
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1645
_journal_paper_doi               10.1039/a909881j
_journal_year                    2000
_chemical_formula_sum            'C71 H53 Cl2 Ir4 N O9 P4'
_chemical_formula_weight         2027.72
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6694(8)
_cell_length_b                   26.479(2)
_cell_length_c                   20.7990(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6960.3(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28587
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    7.848
_exptl_absorpt_correction_T_max  0.0530
_exptl_absorpt_correction_T_min  0.0210
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            gelb
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_F_000             3840
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.000294(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.816
_refine_ls_goodness_of_fit_obs   1.958
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         11402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.816
_refine_ls_restrained_S_obs      1.958
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_obs          0.0554
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0858
_refine_ls_wR_factor_obs         0.0823
_reflns_number_observed          9191
_reflns_number_total             11402
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a909881j.txt
_cod_data_source_block           Compound_2
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6960.4(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009303