N-alkyl functionalised expanded ring N-heterocyclic carbene complexes of rhodium(i) and iridium(i): structural investigations and preliminary catalytic evaluation.
Dunsford, Jay J.; Tromp, Dorette S.; Cavell, Kingsley J.; Elsevier, Cornelis J.; Kariuki, Benson M.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7318–7329; doi:10.1039/c2dt32823b

data_7021125
_publ_section_title
;
 N-alkyl functionalised expanded ring N-heterocyclic carbene complexes of
 rhodium(i) and iridium(i): structural investigations and preliminary
 catalytic evaluation.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7318
_journal_page_last               7329
_journal_paper_doi               10.1039/c2dt32823b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C12 H25 Cl2 I N2'
_chemical_formula_sum            'C12 H25 Cl2 I N2'
_chemical_formula_weight         395.14
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.0834(6)
_cell_length_b                   10.1732(3)
_cell_length_c                   13.7406(3)
_cell_measurement_reflns_used    5458
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      1.62
_cell_volume                     3506.30(15)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXs-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD 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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19185
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.7704
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(7)
_refine_ls_extinction_coef       0.0036(4)
_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_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1186P)^2^+9.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                5458
_reflns_number_total             8832
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt32823b.txt
_cod_data_source_block           kjc1115t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3506.31(15)
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7021125