#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:18:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179809 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/05/7010515.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_7010515
loop_
_publ_author_name
'Connelly, Neil G.'
'Emslie, David J. H.'
'Hayward, Owen D.'
'Orpen, A. Guy'
'Quayle, Michael J.'
_publ_section_title
;
 Redox-active catecholate complexes of rhodium
 hydrotris(pyrazolyl)borates
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              875
_journal_paper_doi               10.1039/b010061g
_journal_year                    2001
_chemical_formula_structural     '[Rh(PPh3)(Tp)(O2C6Cl4)]CH2Cl2'
_chemical_formula_sum            'C40 H39 B Cl6 N6 O2 P Rh'
_chemical_formula_weight         993.16
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.053(4)
_cell_length_b                   14.046(4)
_cell_length_c                   14.439(3)
_cell_measurement_reflns_used    224
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     4269.8(17)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       'ω rotation with narrow frame'
_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  0.0905
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26097
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00051(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.115
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_restrained_S_obs      1.149
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0459
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0252P)²+4.2747P] where where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0932
_refine_ls_wR_factor_obs         0.0779
_reflns_number_observed          3421
_reflns_number_total             5068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b010061g.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+4.2747P] where where
P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+4.2747P] where where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4269.9(17)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7010515
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Rh1 Rh 0.78911(2) 0.2500 0.59525(3) 0.01748(11) Uani 1 d S .
P1 P 0.83677(6) 0.2500 0.44752(9) 0.0193(3) Uani 1 d S .
O1 O 0.72069(10) 0.1542(2) 0.5644(2) 0.0205(5) Uani 1 d . .
N1 N 0.84928(13) 0.1399(2) 0.6351(2) 0.0234(7) Uani 1 d . .
N2 N 0.89289(13) 0.1606(2) 0.7032(2) 0.0256(7) Uani 1 d . .
N3 N 0.8138(2) 0.2500 0.7987(3) 0.0270(11) Uani 1 d S .
N4 N 0.7629(2) 0.2500 0.7377(3) 0.0249(10) Uani 1 d S .
B1 B 0.8834(3) 0.2500 0.7625(5) 0.0281(15) Uani 1 d S .
H1 H 0.9147(27) 0.2500 0.8188(40) 0.050 Uiso 1 d S .
C1 C 0.9221(3) 0.2500 0.4700(4) 0.0336(14) Uani 1 d S .
C2 C 0.9544(2) 0.1649(4) 0.4840(3) 0.058(2) Uani 1 d . .
H2A H 0.9337(2) 0.1059(4) 0.4733(3) 0.069 Uiso 1 calc R .
C3 C 1.0176(2) 0.1666(7) 0.5140(4) 0.109(4) Uani 1 d . .
H3A H 1.0391(2) 0.1083(7) 0.5256(4) 0.130 Uiso 1 calc R .
C4 C 1.0487(4) 0.2500 0.5267(6) 0.131(7) Uani 1 d S .
H4A H 1.0921(4) 0.2500 0.5445(6) 0.158 Uiso 1 calc SR .
C13 C 0.8228(2) 0.1511(3) 0.3675(2) 0.0245(8) Uani 1 d . .
C14 C 0.8687(2) 0.1258(4) 0.3021(3) 0.0572(15) Uani 1 d . .
H14A H 0.9089(2) 0.1567(4) 0.3020(3) 0.069 Uiso 1 calc R .
C15 C 0.8557(2) 0.0556(4) 0.2372(4) 0.076(2) Uani 1 d . .
H15A H 0.8875(2) 0.0380(4) 0.1938(4) 0.091 Uiso 1 calc R .
C16 C 0.7979(2) 0.0114(3) 0.2345(3) 0.0472(12) Uani 1 d . .
H16A H 0.7897(2) -0.0366(3) 0.1897(3) 0.057 Uiso 1 calc R .
C17 C 0.7519(2) 0.0366(3) 0.2970(3) 0.0352(10) Uani 1 d . .
H17A H 0.7117(2) 0.0059(3) 0.2958(3) 0.042 Uiso 1 calc R .
C18 C 0.7641(2) 0.1071(3) 0.3620(3) 0.0295(9) Uani 1 d . .
H18A H 0.7314(2) 0.1255(3) 0.4037(3) 0.035 Uiso 1 calc R .
C19 C 0.8568(2) 0.0470(3) 0.6121(3) 0.0279(9) Uani 1 d . .
C20 C 0.9066(2) 0.0098(3) 0.6654(3) 0.0350(10) Uani 1 d . .
H20A H 0.9224(2) -0.0535(3) 0.6632(3) 0.042 Uiso 1 calc R .
C21 C 0.9282(2) 0.0818(3) 0.7214(3) 0.0330(10) Uani 1 d . .
C22 C 0.8181(2) -0.0067(3) 0.5437(3) 0.0372(10) Uani 1 d . .
H22A H 0.7865(2) 0.0358(3) 0.5160(3) 0.056 Uiso 1 calc R .
H22B H 0.7965(2) -0.0595(3) 0.5750(3) 0.056 Uiso 1 calc R .
H22C H 0.8458(2) -0.0320(3) 0.4951(3) 0.056 Uiso 1 calc R .
C23 C 0.9807(2) 0.0808(4) 0.7913(3) 0.0496(13) Uani 1 d . .
H23A H 0.9844(2) 0.1438(4) 0.8199(3) 0.074 Uiso 1 calc R .
H23B H 1.0208(2) 0.0646(4) 0.7606(3) 0.074 Uiso 1 calc R .
H23C H 0.9714(2) 0.0333(4) 0.8392(3) 0.074 Uiso 1 calc R .
C24 C 0.7100(3) 0.2500 0.7892(4) 0.0349(14) Uani 1 d S .
C25 C 0.7275(3) 0.2500 0.8830(4) 0.048(2) Uani 1 d S .
H25A H 0.6994(3) 0.2500 0.9345(4) 0.057 Uiso 1 calc SR .
C26 C 0.7921(3) 0.2500 0.8866(4) 0.0370(14) Uani 1 d S .
C27 C 0.6443(2) 0.2500 0.7487(4) 0.047(2) Uani 1 d S .
H27A H 0.6427(7) 0.2941(28) 0.6962(23) 0.071 Uiso 0.50 calc PR .
H27B H 0.6137(4) 0.2702(36) 0.7959(11) 0.071 Uiso 0.50 calc PR .
H27C H 0.6336(10) 0.1857(8) 0.7275(33) 0.071 Uiso 0.50 calc PR .
C28 C 0.8350(3) 0.2500 0.9706(4) 0.049(2) Uani 1 d S .
H28A H 0.8114(8) 0.2263(32) 1.0243(8) 0.074 Uiso 0.50 calc PR .
H28B H 0.8497(18) 0.3150(5) 0.9828(20) 0.074 Uiso 0.50 calc PR .
H28C H 0.8717(12) 0.2087(27) 0.9590(13) 0.074 Uiso 0.50 calc PR .
C38 C 0.5609(2) 0.2005(3) 0.4736(2) 0.0271(9) Uani 1 d . .
C39 C 0.6157(2) 0.1517(3) 0.5017(2) 0.0237(8) Uani 1 d . .
C40 C 0.66889(15) 0.1995(2) 0.5333(2) 0.0186(7) Uani 1 d . .
C50 C 0.1327(3) 0.2500 0.2410(5) 0.083(3) Uani 1 d S .
H50A H 0.1400(3) 0.3069 0.2019(5) 0.100 Uiso 0.50 calc PR .
H50B H 0.1400(3) 0.1931 0.2019(5) 0.100 Uiso 0.50 calc PR .
Cl1 Cl 0.61873(5) 0.02795(7) 0.49785(8) 0.0374(3) Uani 1 d . .
Cl2 Cl 0.49412(4) 0.13803(8) 0.43932(8) 0.0392(3) Uani 1 d . .
Cl3 Cl 0.05425(9) 0.2500 0.27730(11) 0.0520(5) Uani 1 d S .
Cl4 Cl 0.18822(9) 0.2500 0.33127(12) 0.0588(5) Uani 1 d S .
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
O1 Rh1 O1 83.49(13) . 7_565 ?
O1 Rh1 N1 171.90(10) . 7_565 ?
O1 Rh1 N1 90.00(11) 7_565 7_565 ?
O1 Rh1 N1 90.00(11) . . ?
O1 Rh1 N1 171.90(10) 7_565 . ?
N1 Rh1 N1 96.1(2) 7_565 . ?
O1 Rh1 N4 91.61(11) . . ?
O1 Rh1 N4 91.61(10) 7_565 . ?
N1 Rh1 N4 83.75(11) 7_565 . ?
N1 Rh1 N4 83.75(11) . . ?
O1 Rh1 P1 95.96(7) . . ?
O1 Rh1 P1 95.96(7) 7_565 . ?
N1 Rh1 P1 89.48(8) 7_565 . ?
N1 Rh1 P1 89.48(8) . . ?
N4 Rh1 P1 169.84(12) . . ?
O1 Rh1 B1 128.54(9) . . ?
O1 Rh1 B1 128.54(9) 7_565 . ?
N1 Rh1 B1 53.12(9) 7_565 . ?
N1 Rh1 B1 53.12(9) . . ?
N4 Rh1 B1 54.5(2) . . ?
P1 Rh1 B1 115.38(12) . . ?
C1 P1 C13 105.7(2) . 7_565 ?
C1 P1 C13 105.7(2) . . ?
C13 P1 C13 98.7(2) 7_565 . ?
C1 P1 Rh1 104.9(2) . . ?
C13 P1 Rh1 120.20(12) 7_565 . ?
C13 P1 Rh1 120.20(12) . . ?
C40 O1 Rh1 109.7(2) . . ?
C40 O1 O1 61.6(2) . 7_565 ?
Rh1 O1 O1 48.26(7) . 7_565 ?
C19 N1 N2 107.4(3) . . ?
C19 N1 Rh1 136.0(3) . . ?
N2 N1 Rh1 116.5(2) . . ?
C21 N2 N1 109.4(3) . . ?
C21 N2 B1 129.0(4) . . ?
N1 N2 B1 119.0(3) . . ?
C26 N3 N4 109.6(4) . . ?
C26 N3 B1 129.4(5) . . ?
N4 N3 B1 120.9(4) . . ?
C24 N4 N3 106.8(4) . . ?
C24 N4 Rh1 138.8(3) . . ?
N3 N4 Rh1 114.4(3) . . ?
N2 B1 N2 110.0(5) 7_565 . ?
N2 B1 N3 108.1(3) 7_565 . ?
N2 B1 N3 108.1(3) . . ?
N2 B1 Rh1 69.6(2) 7_565 . ?
N2 B1 Rh1 69.6(2) . . ?
N3 B1 Rh1 70.2(3) . . ?
C2 C1 C2 118.7(6) 7_565 . ?
C2 C1 P1 120.5(3) 7_565 . ?
C2 C1 P1 120.5(3) . . ?
C1 C2 C3 119.7(6) . . ?
C4 C3 C2 121.1(8) . . ?
C3 C4 C3 119.8(9) 7_565 . ?
C18 C13 C14 117.7(4) . . ?
C18 C13 P1 121.2(3) . . ?
C14 C13 P1 120.6(3) . . ?
C15 C14 C13 120.0(4) . . ?
C16 C15 C14 121.2(4) . . ?
C15 C16 C17 119.5(4) . . ?
C16 C17 C18 120.0(4) . . ?
C13 C18 C17 121.4(4) . . ?
N1 C19 C20 108.2(4) . . ?
N1 C19 C22 125.9(3) . . ?
C20 C19 C22 125.8(4) . . ?
C21 C20 C19 107.3(4) . . ?
N2 C21 C20 107.7(3) . . ?
N2 C21 C23 122.9(4) . . ?
C20 C21 C23 129.5(4) . . ?
N4 C24 C25 108.5(5) . . ?
N4 C24 C27 123.3(5) . . ?
C25 C24 C27 128.2(5) . . ?
C26 C25 C24 107.4(5) . . ?
N3 C26 C25 107.6(5) . . ?
N3 C26 C28 123.6(5) . . ?
C25 C26 C28 128.8(5) . . ?
C38 C38 C39 119.3(2) 7_565 . ?
C38 C38 Cl2 120.52(13) 7_565 . ?
C39 C38 Cl2 120.2(3) . . ?
C40 C39 C38 121.6(3) . . ?
C40 C39 Cl1 117.7(3) . . ?
C38 C39 Cl1 120.6(3) . . ?
O1 C40 C39 122.6(3) . . ?
O1 C40 C40 118.4(2) . 7_565 ?
C39 C40 C40 119.0(2) . 7_565 ?
Cl3 C50 Cl4 114.3(4) . . ?
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 O1 2.021(2) . ?
Rh1 O1 2.021(2) 7_565 ?
Rh1 N1 2.080(3) 7_565 ?
Rh1 N1 2.080(3) . ?
Rh1 N4 2.129(4) . ?
Rh1 P1 2.3574(14) . ?
Rh1 B1 3.126(6) . ?
P1 C1 1.827(5) . ?
P1 C13 1.831(4) 7_565 ?
P1 C13 1.831(4) . ?
O1 C40 1.340(4) . ?
O1 O1 2.691(5) 7_565 ?
N1 C19 1.355(5) . ?
N1 N2 1.376(4) . ?
N2 C21 1.359(5) . ?
N2 B1 1.533(5) . ?
N3 C26 1.348(6) . ?
N3 N4 1.388(5) . ?
N3 B1 1.556(7) . ?
N4 C24 1.339(6) . ?
B1 N2 1.533(5) 7_565 ?
C1 C2 1.389(5) 7_565 ?
C1 C2 1.390(5) . ?
C2 C3 1.399(7) . ?
C3 C4 1.354(9) . ?
C4 C3 1.354(9) 7_565 ?
C13 C18 1.384(5) . ?
C13 C14 1.398(5) . ?
C14 C15 1.388(6) . ?
C15 C16 1.366(6) . ?
C16 C17 1.370(6) . ?
C17 C18 1.388(5) . ?
C19 C20 1.401(5) . ?
C19 C22 1.487(5) . ?
C20 C21 1.372(6) . ?
C21 C23 1.497(5) . ?
C24 C25 1.403(8) . ?
C24 C27 1.501(7) . ?
C25 C26 1.362(8) . ?
C26 C28 1.512(7) . ?
C38 C38 1.389(8) 7_565 ?
C38 C39 1.403(5) . ?
C38 Cl2 1.729(4) . ?
C39 C40 1.384(5) . ?
C39 Cl1 1.740(4) . ?
C40 C40 1.418(7) 7_565 ?
C50 Cl3 1.733(7) . ?
C50 Cl4 1.751(7) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 B1 N2 N1 -10.3(3) . . . . ?
N4 N1 P1 O1 9.52(10) . 7_565 . . ?
