#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:03:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180001 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/95/7029582.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7029582
loop_
_publ_author_name
'Vuong, Khuong Q.'
'Wong, Chin M.'
'Bhadbhade, Mohan'
'Messerle, Barbara A.'
_publ_section_title
;
 Bi- and tri-metallic Rh and Ir complexes containing click derived bis-
 and tris-(pyrazolyl-1,2,3-triazolyl) N-N' donor ligands and their
 application as catalysts for the dihydroalkoxylation of alkynes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7540
_journal_page_last               7553
_journal_paper_doi               10.1039/c3dt53295j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C20 H20 N10'
_chemical_formula_sum            'C20 H20 N10'
_chemical_formula_weight         400.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   10.140(2)
_cell_length_b                   41.977(8)
_cell_length_c                   4.4970(9)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     1914.1(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'Synchrotron BM'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            20945
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin plates'
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.071(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0246P)²+8.5828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                1630
_reflns_number_total             1695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53295j2.cif
_cod_data_source_block           khuong01_Ligand1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7029582--7029586.cif.
;
_cod_original_cell_volume        1914.1(7)
_cod_database_code               7029582
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.7204(4) 0.7500 0.2349(11) 0.0134(10) Uani 1 2 d S
H1 H 0.6541 0.7500 0.0921 0.016 Uiso 1 2 calc SR
C2 C 0.7687(3) 0.72113(7) 0.3390(7) 0.0126(7) Uani 1 1 d .
C3 C 0.8652(3) 0.72136(8) 0.5572(8) 0.0153(8) Uani 1 1 d .
H3 H 0.8995 0.7022 0.6270 0.018 Uiso 1 1 calc R
C4 C 0.9111(4) 0.7500 0.6721(11) 0.0169(11) Uani 1 2 d S
H4 H 0.9724 0.7500 0.8259 0.020 Uiso 1 2 calc SR
C5 C 0.7245(4) 0.69060(7) 0.1918(8) 0.0177(8) Uani 1 1 d .
H51 H 0.6556 0.6956 0.0495 0.021 Uiso 1 1 calc R
H52 H 0.7982 0.6817 0.0822 0.021 Uiso 1 1 calc R
N1A' N 0.6748(3) 0.66641(6) 0.3990(6) 0.0129(7) Uani 1 1 d .
N2A' N 0.5503(3) 0.66690(7) 0.4895(8) 0.0251(8) Uani 1 1 d .
N3A' N 0.5342(3) 0.64212(7) 0.6662(8) 0.0285(9) Uani 1 1 d .
C4A' C 0.6504(3) 0.62645(8) 0.6890(7) 0.0167(8) Uani 1 1 d .
C5A' C 0.7413(3) 0.64178(7) 0.5193(8) 0.0164(8) Uani 1 1 d .
H5A' H 0.8296 0.6365 0.4923 0.020 Uiso 1 1 calc R
C6 C 0.6613(5) 0.59605(8) 0.8623(8) 0.0270(10) Uani 1 1 d .
H62 H 0.7388 0.5970 0.9885 0.032 Uiso 1 1 calc R
H61 H 0.5847 0.5938 0.9896 0.032 Uiso 1 1 calc R
N1A N 0.6707(3) 0.56848(6) 0.6679(6) 0.0164(7) Uani 1 1 d .
N2A N 0.7880(3) 0.56067(7) 0.5426(7) 0.0221(8) Uani 1 1 d .
C3A C 0.7596(4) 0.53641(8) 0.3628(8) 0.0206(8) Uani 1 1 d .
H3A H 0.8213 0.5257 0.2468 0.025 Uiso 1 1 calc R
C4A C 0.6260(4) 0.52909(8) 0.3705(8) 0.0200(8) Uani 1 1 d .
H4A H 0.5827 0.5132 0.2648 0.024 Uiso 1 1 calc R
C5A C 0.5720(3) 0.55020(8) 0.5662(8) 0.0216(9) Uani 1 1 d .
H5A H 0.4835 0.5517 0.6191 0.026 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C2 121.6(4) . 7_575
C2 C1 H1 119.2 . .
C2 C1 H1 119.2 7_575 .
C3 C2 C1 118.8(3) . .
C3 C2 C5 121.7(3) . .
C1 C2 C5 119.2(3) . .
C2 C3 C4 120.4(3) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C3 119.9(4) . 7_575
C3 C4 H4 120.0 . .
C3 C4 H4 120.0 7_575 .
N1A' C5 C2 114.2(3) . .
N1A' C5 H51 108.7 . .
C2 C5 H51 108.7 . .
N1A' C5 H52 108.7 . .
C2 C5 H52 108.7 . .
H51 C5 H52 107.6 . .
N2A' N1A' C5A' 111.4(3) . .
N2A' N1A' C5 120.7(3) . .
C5A' N1A' C5 127.9(3) . .
N3A' N2A' N1A' 106.9(3) . .
N2A' N3A' C4A' 108.7(3) . .
N3A' C4A' C5A' 108.6(3) . .
N3A' C4A' C6 121.2(3) . .
C5A' C4A' C6 130.1(3) . .
N1A' C5A' C4A' 104.4(3) . .
N1A' C5A' H5A' 127.8 . .
C4A' C5A' H5A' 127.8 . .
N1A C6 C4A' 111.7(3) . .
N1A C6 H62 109.3 . .
C4A' C6 H62 109.3 . .
N1A C6 H61 109.3 . .
C4A' C6 H61 109.3 . .
H62 C6 H61 107.9 . .
C5A N1A N2A 112.0(3) . .
C5A N1A C6 127.7(3) . .
N2A N1A C6 120.0(3) . .
C3A N2A N1A 104.3(3) . .
N2A C3A C4A 111.4(3) . .
N2A C3A H3A 124.3 . .
C4A C3A H3A 124.3 . .
C5A C4A C3A 105.3(3) . .
C5A C4A H4A 127.3 . .
C3A C4A H4A 127.3 . .
N1A C5A C4A 107.0(3) . .
N1A C5A H5A 126.5 . .
C4A C5A H5A 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.388(4) .
C1 C2 1.389(4) 7_575
C1 H1 0.9300 .
C2 C3 1.386(5) .
C2 C5 1.511(4) .
C3 C4 1.389(4) .
C3 H3 0.9300 .
C4 C3 1.389(4) 7_575
C4 H4 0.9300 .
C5 N1A' 1.468(4) .
C5 H51 0.9700 .
C5 H52 0.9700 .
N1A' N2A' 1.327(4) .
N1A' C5A' 1.348(4) .
N2A' N3A' 1.319(4) .
N3A' C4A' 1.353(5) .
C4A' C5A' 1.359(5) .
C4A' C6 1.499(5) .
C5A' H5A' 0.9300 .
C6 N1A 1.454(4) .
C6 H62 0.9700 .
C6 H61 0.9700 .
N1A C5A 1.342(5) .
N1A N2A 1.356(4) .
N2A C3A 1.332(5) .
C3A C4A 1.389(5) .
C3A H3A 0.9300 .
C4A C5A 1.364(5) .
C4A H4A 0.9300 .
C5A H5A 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C2 C1 C2 C3 1.6(6) 7_575 .
C2 C1 C2 C5 -172.6(3) 7_575 .
C1 C2 C3 C4 1.0(5) . .
C5 C2 C3 C4 175.0(3) . .
C2 C3 C4 C3 -3.4(6) . 7_575
C3 C2 C5 N1A' 57.4(4) . .
C1 C2 C5 N1A' -128.6(4) . .
C2 C5 N1A' N2A' 84.5(4) . .
C2 C5 N1A' C5A' -95.9(4) . .
C5A' N1A' N2A' N3A' -1.1(4) . .
C5 N1A' N2A' N3A' 178.5(3) . .
N1A' N2A' N3A' C4A' 1.0(4) . .
N2A' N3A' C4A' C5A' -0.5(4) . .
N2A' N3A' C4A' C6 -176.5(3) . .
N2A' N1A' C5A' C4A' 0.8(4) . .
C5 N1A' C5A' C4A' -178.8(3) . .
N3A' C4A' C5A' N1A' -0.1(4) . .
C6 C4A' C5A' N1A' 175.4(3) . .
N3A' C4A' C6 N1A 105.1(4) . .
C5A' C4A' C6 N1A -69.9(5) . .
C4A' C6 N1A C5A -92.2(4) . .
C4A' C6 N1A N2A 80.7(4) . .
C5A N1A N2A C3A -1.1(4) . .
C6 N1A N2A C3A -175.1(3) . .
N1A N2A C3A C4A 0.7(4) . .
N2A C3A C4A C5A 0.0(4) . .
N2A N1A C5A C4A 1.2(4) . .
C6 N1A C5A C4A 174.5(3) . .
C3A C4A C5A N1A -0.7(4) . .
