#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/22/7012208.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_7012208
loop_
_publ_author_name
'Braunstein, Pierre'
'Heaton, Brian T.'
'Jacob, Chacko'
'Manzi, Lucia'
'Morise, Xavier'
_publ_section_title
;
 Rhodium complexes containing the hybrid P,O ligand PPh2NHC(O)Me or its
 anion, [PPh2NC(O)Me]--
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1396
_journal_page_last               1401
_journal_paper_doi               10.1039/b208735a
_journal_year                    2003
_chemical_formula_moiety         'C16 H16 N O2 P Cl3 Rh'
_chemical_formula_sum            'C16 H16 Cl3 N O2 P Rh'
_chemical_formula_weight         494.55
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.916(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5442(2)
_cell_length_b                   16.4222(4)
_cell_length_c                   13.2981(2)
_cell_measurement_reflns_used    17433
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.4
_cell_volume                     2031.57(10)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
180 frames, 30 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 25 mm.
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17433
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.841
_refine_diff_density_min         -1.368
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/esd_mean        0.002
_refine_ls_shift/su_max          0.053
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/(σ²(Fo²)+0.0016 Fo⁴)+4.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.072
_refine_ls_wR_factor_ref         0.070
_reflns_number_gt                3550
_reflns_number_total             4744
_reflns_threshold_expression     >3.0σ(I)
_cod_data_source_file            b208735a.txt
_cod_data_source_block           st198
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0016
Fo^4^)+4.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0016 Fo^4^)+4.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2031.6(2)
_cod_original_formula_sum        'C16 H16 N O2 P Cl3 Rh'
_cod_database_code               7012208
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
RH 0.83869(4) 0.17676(2) 0.31911(3) 0.0403(2) Uani ? ? Rh
CL1 0.7843(2) 0.14092(9) 0.1418(1) 0.0540(7) Uani ? ? Cl
C1 0.6660(6) 0.1498(3) 0.3413(4) 0.052(3) Uani ? ? C
O1 0.5549(5) 0.1338(3) 0.3569(4) 0.077(3) Uani ? ? O
P 0.9166(1) 0.22097(7) 0.47624(9) 0.0375(5) Uani ? ? P
C2 0.8371(5) 0.3113(3) 0.5173(4) 0.039(2) Uani ? ? C
C3 0.8732(6) 0.3877(3) 0.4872(4) 0.050(2) Uani ? ? C
C4 0.8023(6) 0.4558(3) 0.5097(5) 0.055(3) Uani ? ? C
C5 0.6952(7) 0.4483(4) 0.5635(5) 0.065(3) Uani ? ? C
C6 0.6554(7) 0.3729(4) 0.5928(5) 0.070(3) Uani ? ? C
C7 0.7267(6) 0.3042(3) 0.5703(4) 0.056(3) Uani ? ? C
C8 0.9475(5) 0.1538(3) 0.5858(4) 0.042(2) Uani ? ? C
C9 1.0128(6) 0.1824(3) 0.6840(4) 0.047(2) Uani ? ? C
C10 1.0475(6) 0.1289(4) 0.7662(4) 0.051(3) Uani ? ? C
C11 1.0172(7) 0.0475(4) 0.7531(5) 0.060(3) Uani ? ? C
C12 0.9495(9) 0.0191(4) 0.6563(5) 0.068(4) Uani ? ? C
C13 0.9145(7) 0.0712(3) 0.5715(5) 0.057(3) Uani ? ? C
N 1.0868(4) 0.2532(3) 0.4695(3) 0.042(2) Uani ? ? N
C14 1.1279(5) 0.2427(3) 0.3807(4) 0.047(2) Uani ? ? C
C15 1.2750(6) 0.2677(5) 0.3732(5) 0.063(3) Uani ? ? C
O2 1.0443(4) 0.2105(2) 0.3036(3) 0.051(2) Uani ? ? O
C16 0.883(1) 0.3940(8) 0.179(1) 0.147(8) Uani ? ? C
CL2 1.0446(5) 0.4315(3) 0.2438(4) 0.188(3) Uani ? ? Cl
CL3 0.8555(6) 0.4103(3) 0.0494(3) 0.191(4) Uani ? ? Cl
H1 1.0335 0.2388 0.6944 0.0618 Uiso calc C9 H
H2 1.0928 0.1489 0.8326 0.0683 Uiso calc C10 H
H3 1.0424 0.0110 0.8097 0.0786 Uiso calc C11 H
H4 0.9263 -0.0371 0.6475 0.0975 Uiso calc C12 H
H5 0.8691 0.0509 0.5054 0.0807 Uiso calc C13 H
H6 0.9476 0.3931 0.4506 0.0645 Uiso calc C3 H
H7 0.8271 0.5080 0.4882 0.0760 Uiso calc C4 H
H8 0.6483 0.4957 0.5805 0.0854 Uiso calc C5 H
H9 0.5796 0.3680 0.6282 0.0874 Uiso calc C6 H
H10 0.7005 0.2521 0.5909 0.0708 Uiso calc C7 H
H11 1.2879 0.2564 0.3058 0.0847 Uiso calc C15 H
H12 1.2869 0.3244 0.3866 0.0847 Uiso calc C15 H
H13 1.3440 0.2382 0.4223 0.0847 Uiso calc C15 H
H14 0.8088 0.4200 0.2035 0.2077 Uiso calc C16 H
H15 0.8809 0.3371 0.1907 0.2077 Uiso calc C16 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1
Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1
Rh ? -1.287 0.919 International_Tables_Vol_IV_Table_2.3.1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
CL1 RH C1 95.6(2) . . . ?
CL1 RH P 170.88(6) . . . ?
CL1 RH O2 88.2(1) . . . ?
C1 RH P 93.1(2) . . . ?
C1 RH O2 176.2(2) . . . ?
P RH O2 83.1(1) . . . ?
C2 P C8 105.2(2) . . . ?
C2 P N 103.1(2) . . . ?
C8 P N 104.1(2) . . . ?
P C2 C3 120.6(4) . . . ?
P C2 C7 119.9(4) . . . ?
C3 C2 C7 119.1(5) . . . ?
C2 C3 C4 120.5(5) . . . ?
C3 C4 C5 120.0(5) . . . ?
C4 C5 C6 120.7(5) . . . ?
C5 C6 C7 119.4(6) . . . ?
C2 C7 C6 120.3(5) . . . ?
P C8 C9 120.6(4) . . . ?
P C8 C13 119.6(4) . . . ?
C9 C8 C13 119.6(5) . . . ?
C8 C9 C10 120.2(5) . . . ?
C9 C10 C11 120.8(5) . . . ?
C10 C11 C12 119.2(5) . . . ?
C11 C12 C13 121.4(6) . . . ?
C8 C13 C12 118.7(6) . . . ?
P N C14 118.0(4) . . . ?
N C14 C15 119.4(5) . . . ?
N C14 O2 120.9(5) . . . ?
C15 C14 O2 119.6(5) . . . ?
CL2 C16 CL3 112.1(7) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
RH CL1 2.372(1) . . ?
RH C1 1.794(7) . . ?
RH P 2.180(1) . . ?
RH O2 2.094(4) . . ?
C1 O1 1.155(7) . . ?
P C2 1.806(5) . . ?
P C8 1.799(5) . . ?
P N 1.730(4) . . ?
C2 C3 1.383(7) . . ?
C2 C7 1.397(7) . . ?
C3 C4 1.374(8) . . ?
C4 C5 1.377(9) . . ?
C5 C6 1.378(9) . . ?
C6 C7 1.384(8) . . ?
C8 C9 1.396(7) . . ?
C8 C13 1.396(7) . . ?
C9 C10 1.384(7) . . ?
C10 C11 1.370(9) . . ?
C11 C12 1.39(1) . . ?
C12 C13 1.395(8) . . ?
N C14 1.337(6) . . ?
C14 C15 1.487(8) . . ?
C14 O2 1.265(6) . . ?
C16 CL2 1.70(1) . . ?
C16 CL3 1.70(2) . . ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
