Stable crystalline annulated diaminocarbenes: coordination with rhodium(i), iridium(i) and catalytic hydroformylation studies
Dastgir, Sarim; Coleman, Karl S.; Cowley, Andrew R.; Green, Malcolm L. H.; Dalton Transactions  (2009) 7203–; doi:10.1039/b905729c

data_7001958
_publ_section_title
;
 Stable crystalline annulated diaminocarbenes: coordination with
 rhodium(i), iridium(i) and catalytic hydroformylation studies
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              7203
_journal_paper_doi               10.1039/b905729c
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C50 H59 Ir N3, F6 P, C H2 Cl2 '
_chemical_formula_sum            'C51 H61 Cl2 F6 Ir N3 P'
_chemical_formula_weight         1124.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.0100(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6624(3)
_cell_length_b                   15.6085(2)
_cell_length_c                   16.6277(3)
_cell_measurement_reflns_used    22099
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     4843.52(13)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'CRYSTALS (Watkin et al, 2001)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22099
_diffrn_reflns_theta_full        27.479
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         5.096
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.961
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       ' fragment '
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.48
_refine_ls_abs_structure_details 'Flack, 4865 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.384(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9261
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.009076
_refine_ls_structure_factor_coef F
_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:
1.68 -0.207 0.695
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0525
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0423
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                9261
_reflns_number_total             10370
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b905729c.txt
_cod_data_source_block           (COD)Ir(BIAN-SIPr)(Py)_8b
_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 
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_sum        ' C51 H61 Cl2 F6 Ir N3 P '
_cod_database_code               7001958