#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:53:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179710 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/13/7001345.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_7001345
loop_
_publ_author_name
'Hallett, Andrew J.'
'Anderson, Kirsty M.'
'Connelly, Neil G.'
'Haddow, Mairi F.'
_publ_section_title
;
 Bonding modes, structures and fluxionality in rhodium and iridium
 tris(3,5-dimethylpyrazolyl)methane diene complexes
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              4181
_journal_page_last               4189
_journal_paper_doi               10.1039/b900817a
_journal_year                    2009
_chemical_formula_moiety         'C22 H32 N6 Rh, F6 P'
_chemical_formula_sum            'C22 H32 F6 N6 P Rh'
_chemical_formula_weight         628.42
_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                   14.481(3)
_cell_length_b                   12.148(2)
_cell_length_c                   15.203(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2674.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD area detector'
_diffrn_measurement_method       'ω scans with narrow frames'
_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  0.3124
_diffrn_reflns_av_sigmaI/netI    0.2011
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13824
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.436149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.490
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2148
_refine_ls_R_factor_gt           0.0830
_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)+(0.0975P)²+35.9544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2642
_reflns_number_gt                1096
_reflns_number_total             2475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900817a.txt
_cod_data_source_block           4+
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2674.5(9)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7001345
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.04326(10) 0.2500 0.24447(12) 0.0265(5) Uani 1 2 d S . .
P1 P -0.1398(4) 0.2500 0.7950(4) 0.0347(15) Uani 1 2 d S . .
F1 F -0.0310(8) 0.2500 0.8020(9) 0.053(4) Uani 1 2 d S . .
F2 F -0.2502(9) 0.2500 0.7886(9) 0.054(4) Uani 1 2 d S . .
F3 F -0.1447(6) 0.1579(7) 0.8696(6) 0.046(2) Uani 1 1 d . . .
F4 F -0.1355(7) 0.1564(8) 0.7203(6) 0.065(3) Uani 1 1 d . . .
N1 N -0.0569(7) 0.1306(9) 0.3016(8) 0.031(3) Uani 1 1 d . . .
N2 N -0.0845(7) 0.1530(10) 0.3857(8) 0.029(3) Uani 1 1 d . . .
N5 N 0.1001(10) 0.2500 0.3733(10) 0.023(4) Uani 1 2 d S . .
N6 N 0.0434(11) 0.2500 0.4445(9) 0.022(3) Uani 1 2 d S . .
C1 C 0.1321(11) 0.1423(13) 0.1828(9) 0.041(4) Uani 1 1 d . . .
H1A H 0.1985 0.1618 0.1853 0.049 Uiso 1 1 calc R . .
H1B H 0.1206 0.0631 0.1935 0.049 Uiso 1 1 calc R . .
C2 C 0.0809(10) 0.1906(12) 0.1130(10) 0.038(4) Uani 1 1 d . . .
C3 C 0.0340(12) 0.1285(14) 0.0430(10) 0.057(5) Uani 1 1 d . . .
H3A H 0.0763 0.1184 -0.0067 0.086 Uiso 1 1 calc R . .
H3B H -0.0206 0.1695 0.0233 0.086 Uiso 1 1 calc R . .
H3C H 0.0149 0.0565 0.0656 0.086 Uiso 1 1 calc R . .
C5 C -0.0564(12) 0.2500 0.4320(13) 0.026(5) Uani 1 2 d S . .
H5A H -0.0866 0.2500 0.4911 0.031 Uiso 1 2 calc SR . .
C6 C -0.0885(12) -0.0151(14) 0.1910(11) 0.054(5) Uani 1 1 d . . .
H6A H -0.0464 0.0288 0.1547 0.081 Uiso 1 1 calc R . .
H6B H -0.1490 -0.0194 0.1623 0.081 Uiso 1 1 calc R . .
H6C H -0.0633 -0.0895 0.1982 0.081 Uiso 1 1 calc R . .
C7 C -0.0989(10) 0.0379(12) 0.2795(10) 0.036(4) Uani 1 1 d . . .
C8 C -0.1521(10) 0.0013(12) 0.3492(12) 0.043(4) Uani 1 1 d . . .
H8A H -0.1886 -0.0637 0.3497 0.052 Uiso 1 1 calc R . .
C9 C -0.1435(10) 0.0740(13) 0.4166(10) 0.038(4) Uani 1 1 d . . .
C10 C -0.1861(11) 0.0769(14) 0.5055(11) 0.054(5) Uani 1 1 d . . .
H10A H -0.2262 0.0127 0.5131 0.081 Uiso 1 1 calc R . .
H10B H -0.2227 0.1443 0.5118 0.081 Uiso 1 1 calc R . .
H10C H -0.1374 0.0757 0.5503 0.081 Uiso 1 1 calc R . .
C11 C 0.2712(13) 0.2500 0.3538(16) 0.051(7) Uani 1 2 d S . .
H11A H 0.2534 0.2500 0.2916 0.076 Uiso 1 2 calc SR . .
H11B H 0.3080 0.1841 0.3665 0.076 Uiso 0.50 1 calc PR . .
H11C H 0.3080 0.3159 0.3665 0.076 Uiso 0.50 1 calc PR . .
C12 C 0.1836(11) 0.2500 0.4116(14) 0.027(5) Uani 1 2 d S . .
C13 C 0.1797(13) 0.2500 0.5010(15) 0.033(5) Uani 1 2 d S . .
H13A H 0.2305 0.2500 0.5406 0.039 Uiso 1 2 calc SR . .
C14 C 0.0852(14) 0.2500 0.5228(14) 0.031(5) Uani 1 2 d S . .
C15 C 0.0385(15) 0.2500 0.6085(13) 0.043(6) Uani 1 2 d S . .
H15A H -0.0285 0.2500 0.5995 0.064 Uiso 1 2 calc SR . .
H15B H 0.0564 0.3159 0.6415 0.064 Uiso 0.50 1 calc PR . .
H15C H 0.0564 0.1841 0.6415 0.064 Uiso 0.50 1 calc PR . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 '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
_geom_angle_publ_flag
C1 Rh1 C1 78.8(9) 8_565 . ?
C1 Rh1 N5 100.2(5) 8_565 . ?
C1 Rh1 N5 100.2(5) . . ?
C1 Rh1 C2 68.8(6) 8_565 . ?
C1 Rh1 C2 38.9(5) . . ?
N5 Rh1 C2 138.0(5) . . ?
C1 Rh1 C2 38.9(5) 8_565 8_565 ?
C1 Rh1 C2 68.8(6) . 8_565 ?
N5 Rh1 C2 138.0(5) . 8_565 ?
C2 Rh1 C2 38.4(8) . 8_565 ?
C1 Rh1 N1 175.9(5) 8_565 . ?
C1 Rh1 N1 99.8(5) . . ?
N5 Rh1 N1 83.8(4) . . ?
C2 Rh1 N1 107.6(5) . . ?
C2 Rh1 N1 137.0(5) 8_565 . ?
C1 Rh1 N1 99.8(5) 8_565 8_565 ?
C1 Rh1 N1 175.9(5) . 8_565 ?
N5 Rh1 N1 83.8(4) . 8_565 ?
C2 Rh1 N1 137.0(5) . 8_565 ?
C2 Rh1 N1 107.6(5) 8_565 8_565 ?
N1 Rh1 N1 81.2(6) . 8_565 ?
F1 P1 F3 89.8(5) . 8_565 ?
F1 P1 F3 89.8(5) . . ?
F3 P1 F3 89.1(7) 8_565 . ?
F1 P1 F2 179.6(8) . . ?
F3 P1 F2 89.9(5) 8_565 . ?
F3 P1 F2 89.9(5) . . ?
F1 P1 F4 90.5(6) . . ?
F3 P1 F4 179.5(6) 8_565 . ?
F3 P1 F4 90.5(5) . . ?
F2 P1 F4 89.8(6) . . ?
F1 P1 F4 90.5(6) . 8_565 ?
F3 P1 F4 90.5(5) 8_565 8_565 ?
F3 P1 F4 179.5(6) . 8_565 ?
F2 P1 F4 89.8(6) . 8_565 ?
F4 P1 F4 89.9(8) . 8_565 ?
C7 N1 N2 105.8(12) . . ?
C7 N1 Rh1 139.0(11) . . ?
N2 N1 Rh1 115.2(8) . . ?
N1 N2 C9 111.3(11) . . ?
N1 N2 C5 122.7(12) . . ?
C9 N2 C5 125.9(13) . . ?
C12 N5 N6 101.5(15) . . ?
C12 N5 Rh1 138.5(13) . . ?
N6 N5 Rh1 120.0(11) . . ?
C14 N6 N5 115.8(16) . . ?
C14 N6 C5 124.4(16) . . ?
N5 N6 C5 119.7(14) . . ?
C2 C1 Rh1 75.6(9) . . ?
C1 C2 C2 114.4(9) . 8_565 ?
C1 C2 C3 124.8(14) . . ?
C2 C2 C3 120.8(9) 8_565 . ?
C1 C2 Rh1 65.5(8) . . ?
C2 C2 Rh1 70.8(4) 8_565 . ?
C3 C2 Rh1 135.5(11) . . ?
N2 C5 N2 110.8(16) . 8_565 ?
N2 C5 N6 110.3(10) . . ?
N2 C5 N6 110.3(10) 8_565 . ?
N1 C7 C8 109.6(14) . . ?
N1 C7 C6 123.2(15) . . ?
C8 C7 C6 127.2(15) . . ?
C9 C8 C7 108.5(14) . . ?
C8 C9 N2 104.7(13) . . ?
C8 C9 C10 131.6(15) . . ?
N2 C9 C10 123.7(14) . . ?
N5 C12 C13 113.3(17) . . ?
N5 C12 C11 119.6(19) . . ?
C13 C12 C11 127.1(17) . . ?
C12 C13 C14 106.0(18) . . ?
N6 C14 C13 103.3(18) . . ?
N6 C14 C15 125.6(18) . . ?
C13 C14 C15 131(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 2.061(15) 8_565 ?
Rh1 C1 2.061(15) . ?
Rh1 N5 2.125(16) . ?
Rh1 C2 2.193(15) . ?
Rh1 C2 2.193(15) 8_565 ?
Rh1 N1 2.228(12) . ?
Rh1 N1 2.228(12) 8_565 ?
P1 F1 1.578(12) . ?
P1 F3 1.594(9) 8_565 ?
P1 F3 1.594(9) . ?
P1 F2 1.603(14) . ?
P1 F4 1.609(10) . ?
P1 F4 1.609(10) 8_565 ?
N1 C7 1.323(17) . ?
N1 N2 1.366(15) . ?
N2 C9 1.368(17) . ?
N2 C5 1.432(15) . ?
N5 C12 1.34(2) . ?
N5 N6 1.36(2) . ?
N6 C14 1.34(2) . ?
N6 C5 1.46(2) . ?
C1 C2 1.42(2) . ?
C2 C2 1.44(3) 8_565 ?
C2 C3 1.471(19) . ?
C5 N2 1.432(15) 8_565 ?
C6 C7 1.50(2) . ?
C7 C8 1.38(2) . ?
C8 C9 1.36(2) . ?
C9 C10 1.49(2) . ?
C11 C12 1.54(3) . ?
C12 C13 1.36(3) . ?
C13 C14 1.41(3) . ?
C14 C15 1.47(3) . ?
