#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:21:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179839 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/35/7013548.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_7013548
loop_
_publ_author_name
'Burrows, Andrew D.'
'Mahon, Mary F.'
'Varrone, Maurizio'
_publ_section_title
;
 The synthesis and late transition metal chemistry of 7-aza-N-indolyl
 phosphines and the activity of their palladium complexes in CO?ethene
 co-polymerisation
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4718
_journal_paper_doi               10.1039/b309882f
_journal_year                    2003
_chemical_formula_sum            'C16 H13 Cl N4 O P Rh'
_chemical_formula_weight         446.63
_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                 99.2540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.71300(10)
_cell_length_b                   11.0150(2)
_cell_length_c                   17.8380(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1689.70(4)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29040
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0113(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0217
_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
[1.00000+0.00000exp(0.00(sinθ/λ)²)]/
[σ²(Fo²)+0.0000+1.5445*P+(0.0351P)²+0.0000sinθ/λ]
where P = 0.00000Fo² + 1.00000Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                3675
_reflns_number_total             3794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309882f.txt
_cod_data_source_block           compound3b_h01adb4
_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.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' 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_sg_symbol_H-M      P21/c
_cod_database_code               7013548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.184388(14) 0.215684(11) 0.273641(7) 0.01613(8) Uani 1 1 d . . .
P1 P 0.08027(5) 0.26265(4) 0.15886(2) 0.01670(10) Uani 1 1 d . . .
Cl2 Cl 0.31314(5) 0.15820(4) 0.39520(2) 0.02309(11) Uani 1 1 d . . .
C3 C 0.4334(2) -0.10875(19) 0.20516(12) 0.0327(4) Uani 1 1 d . . .
H3 H 0.4993 -0.1730 0.2279 0.039 Uiso 1 1 d R . .
N3 N 0.12093(17) 0.39359(14) 0.11655(9) 0.0203(3) Uani 1 1 d . . .
N4 N -0.11426(17) 0.25920(15) 0.13310(9) 0.0208(3) Uani 1 1 d . . .
O1 O 0.03852(19) 0.42672(15) 0.33848(9) 0.0382(4) Uani 1 1 d . . .
N2 N 0.15848(18) 0.15870(14) 0.10545(8) 0.0212(3) Uani 1 1 d . . .
C4 C 0.4006(2) -0.10314(18) 0.12673(12) 0.0297(4) Uani 1 1 d . . .
H4 H 0.4419 -0.1617 0.0954 0.036 Uiso 1 1 d R . .
C16 C -0.2112(2) 0.19497(18) 0.17420(11) 0.0249(4) Uani 1 1 d . . .
H16 H -0.1916 0.1545 0.2225 0.030 Uiso 1 1 d R . .
N1 N 0.28207(17) 0.06867(14) 0.22094(8) 0.0195(3) Uani 1 1 d . . .
C6 C 0.2390(2) 0.03284(19) 0.01945(11) 0.0290(4) Uani 1 1 d . . .
H6 H 0.2467 0.0035 -0.0305 0.035 Uiso 1 1 d R . .
C12 C 0.0509(2) 0.50442(17) 0.12873(11) 0.0267(4) Uani 1 1 d . . .
H12 H -0.0490 0.5233 0.1419 0.032 Uiso 1 1 d R . .
C1 C 0.0950(2) 0.34640(18) 0.31305(10) 0.0238(4) Uani 1 1 d . . .
C8 C 0.25043(19) 0.07057(15) 0.14505(10) 0.0185(3) Uani 1 1 d . . .
C13 C -0.2045(2) 0.29988(19) 0.06590(11) 0.0263(4) Uani 1 1 d . . .
H13 H -0.1784 0.3450 0.0237 0.032 Uiso 1 1 d R . .
C15 C -0.3573(2) 0.1969(2) 0.13386(13) 0.0307(4) Uani 1 1 d . . .
H15 H -0.4535 0.1619 0.1430 0.037 Uiso 1 1 d R . .
C2 C 0.3739(2) -0.02300(18) 0.25077(11) 0.0271(4) Uani 1 1 d . . .
H2 H 0.4001 -0.0312 0.3049 0.033 Uiso 1 1 d R . .
C5 C 0.3035(2) -0.01026(17) 0.09411(11) 0.0228(4) Uani 1 1 d . . .
C14 C -0.3532(2) 0.2636(2) 0.06579(12) 0.0299(4) Uani 1 1 d . . .
H14 H -0.4467 0.2765 0.0302 0.036 Uiso 1 1 d R . .
C7 C 0.1537(2) 0.13333(19) 0.02775(10) 0.0280(4) Uani 1 1 d . . .
H7 H 0.1011 0.1753 -0.0162 0.034 Uiso 1 1 d R . .
C9 C 0.2706(2) 0.41922(19) 0.10214(12) 0.0284(4) Uani 1 1 d . . .
H9 H 0.3537 0.3672 0.0925 0.034 Uiso 1 1 d R . .
C11 C 0.1513(3) 0.59483(18) 0.11998(11) 0.0309(4) Uani 1 1 d . . .
H11 H 0.1432 0.6816 0.1230 0.037 Uiso 1 1 d R . .
C10 C 0.2904(2) 0.5410(2) 0.10309(12) 0.0325(4) Uani 1 1 d . . .
H10 H 0.3762 0.5913 0.0949 0.039 Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 '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'
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 N1 176.30(7) . . ?
C1 Rh1 P1 92.05(6) . . ?
N1 Rh1 P1 84.27(4) . . ?
C1 Rh1 Cl2 91.54(6) . . ?
N1 Rh1 Cl2 92.12(4) . . ?
P1 Rh1 Cl2 175.852(16) . . ?
N4 P1 N3 99.87(8) . . ?
N4 P1 N2 107.97(8) . . ?
N3 P1 N2 101.11(8) . . ?
N4 P1 Rh1 120.21(6) . . ?
N3 P1 Rh1 122.67(6) . . ?
N2 P1 Rh1 102.96(5) . . ?
C4 C3 C2 121.49(18) . . ?
C12 N3 C9 107.19(16) . . ?
C12 N3 P1 123.21(12) . . ?
C9 N3 P1 121.52(13) . . ?
C16 N4 C13 107.96(15) . . ?
C16 N4 P1 122.38(13) . . ?
C13 N4 P1 129.03(13) . . ?
C8 N2 C7 106.70(15) . . ?
C8 N2 P1 116.05(12) . . ?
C7 N2 P1 137.23(13) . . ?
C3 C4 C5 117.88(18) . . ?
C15 C16 N4 107.97(18) . . ?
C8 N1 C2 115.16(15) . . ?
C8 N1 Rh1 113.89(11) . . ?
C2 N1 Rh1 130.91(13) . . ?
C7 C6 C5 107.92(17) . . ?
C11 C12 N3 108.64(17) . . ?
O1 C1 Rh1 178.92(18) . . ?
N1 C8 N2 122.53(15) . . ?
N1 C8 C5 127.59(16) . . ?
N2 C8 C5 109.87(15) . . ?
C14 C13 N4 108.21(18) . . ?
C16 C15 C14 108.04(18) . . ?
N1 C2 C3 121.98(18) . . ?
C4 C5 C8 115.89(17) . . ?
C4 C5 C6 138.46(18) . . ?
C8 C5 C6 105.63(16) . . ?
C13 C14 C15 107.82(17) . . ?
C6 C7 N2 109.87(17) . . ?
C10 C9 N3 108.61(18) . . ?
C12 C11 C10 107.84(18) . . ?
C9 C10 C11 107.69(18) . . ?
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 1.8305(19) . ?
Rh1 N1 2.1184(15) . ?
Rh1 P1 2.1646(4) . ?
Rh1 Cl2 2.3620(4) . ?
P1 N4 1.6837(16) . ?
P1 N3 1.6915(15) . ?
P1 N2 1.7006(15) . ?
C3 C4 1.384(3) . ?
C3 C2 1.399(3) . ?
N3 C12 1.397(2) . ?
N3 C9 1.398(2) . ?
N4 C16 1.397(2) . ?
N4 C13 1.397(2) . ?
O1 C1 1.141(2) . ?
N2 C8 1.379(2) . ?
N2 C7 1.408(2) . ?
C4 C5 1.394(3) . ?
C16 C15 1.358(3) . ?
N1 C8 1.338(2) . ?
N1 C2 1.344(2) . ?
C6 C7 1.355(3) . ?
C6 C5 1.440(3) . ?
C12 C11 1.351(3) . ?
C8 C5 1.403(2) . ?
C13 C14 1.355(3) . ?
C15 C14 1.425(3) . ?
C9 C10 1.353(3) . ?
C11 C10 1.425(3) . ?
