Controlling the Coordination Mode of 1,4,7-Triazacyclononane Complexes of Rhodium and Iridium and Evaluating Their Behavior as Phenylacetylene Polymerization Catalysts
Gott, Andrew L.; McGowan, Patrick C.; Temple, Claire N.; Organometallics 27 (2008) 2852–; doi:10.1021/om800180a

data_4071476
_publ_section_title
;
 Controlling the Coordination Mode of 1,4,7-Triazacyclononane Complexes of
 Rhodium and Iridium and Evaluating Their Behavior as Phenylacetylene
 Polymerization Catalysts
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2852
_journal_paper_doi               10.1021/om800180a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C28 H51 Cl2 N3 Rh2'
_chemical_formula_weight         706.44
_chemical_name_common            in_paper_10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 115.481(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5750(1)
_cell_length_b                   19.6800(3)
_cell_length_c                   19.2950(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2939.42(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'WC (Thornton-Pett, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
    Detector set at 30mm from sample with different 2theta offsets 
    1 degree phi exposures for chi=0 degree settings
    1 degree omega exposures for chi=90 degree settings
;
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40211
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.056
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+18.2333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                5793
_reflns_number_total             6689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800180a-file001.cif
_cod_data_source_block           c:\x-rays~1\unfini~1\ct152b\shelxl
_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_cell_volume        2939.41(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4071476