#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/42/2004292.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004292
loop_
_publ_author_name
'Stammler, H.-G.'
'Jutzi, P.'
'Neumann, B.'
'Kristen, M. O.'
'Hölscher, H.'
_publ_section_title
;
 Intramolecular Coordination of the Dimethylamino Group in a
 Rhodium--Oxalate Complex with the
 1-[2-(Dimethylamino)ethyl]-2,3,4,5-tetramethylcyclopentadienyl Ligand
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2494
_journal_page_last               2496
_journal_paper_doi               10.1107/S0108270195006871
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C15 H22 N O4 Rh'
_chemical_formula_weight         383.25
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.785(5)
_cell_length_b                   9.265(4)
_cell_length_c                   12.881(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      9.8
_cell_measurement_theta_min      3.2
_cell_volume                     1513.1(10)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'P3 Data Collection Program (Siemens, 1989)'
_computing_data_reduction        SHELXTL-Plus
_computing_molecular_graphics    SHELXTL-Plus
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P2₁'
_diffrn_measurement_method       Wyckoff
_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  0.1007
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3467
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        .0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   'semi-empirical via \y scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       needles
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .748
_refine_diff_density_min         -.915
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.368
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_obs          0.0605
_refine_ls_shift/esd_max         -0.084
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0500P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1694
_refine_ls_wR_factor_obs         0.1147
_reflns_number_observed          2051
_reflns_number_total             3303
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1162.cif
_cod_data_source_block           CpRhoxalate
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2004292
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Rh1 1 0.02727(5) 0.10056(7) 0.26553(5) 0.0179(2) Uani d . Rh
O1 1 -0.0297(4) -0.0699(6) 0.1682(4) 0.0236(13) Uani d . O
O2 1 0.0583(4) -0.0740(6) 0.3665(4) 0.0251(13) Uani d . O
O3 1 -0.0654(5) -0.3046(7) 0.1722(4) 0.0324(14) Uani d . O
O4 1 0.0485(5) -0.3140(6) 0.3734(4) 0.0323(14) Uani d . O
N1 1 -0.1321(5) 0.1330(6) 0.3061(5) 0.0196(14) Uani d . N
C1 1 0.1156(6) 0.2737(8) 0.3400(6) 0.021(2) Uani d . C
C2 1 0.1847(6) 0.1879(9) 0.2821(6) 0.025(2) Uani d . C
C3 1 0.1438(6) 0.1951(9) 0.1748(6) 0.023(2) Uani d . C
C4 1 0.0462(6) 0.2777(9) 0.1650(6) 0.023(2) Uani d . C
C5 1 0.0294(7) 0.3263(8) 0.2687(6) 0.021(2) Uani d . C
C6 1 0.1350(7) 0.3048(10) 0.4561(6) 0.036(2) Uani d . C
H6A 1 0.2010(24) 0.2590(50) 0.4864(10) 0.054 Uiso calc R H
H6B 1 0.0764(23) 0.2664(54) 0.4899(9) 0.054 Uiso calc R H
H6C 1 0.1400(44) 0.4094(10) 0.4673(6) 0.054 Uiso calc R H
C7 1 0.2826(6) 0.1134(12) 0.3300(6) 0.037(2) Uani d . C
H7A 1 0.2649(9) 0.0439(48) 0.3824(34) 0.056 Uiso calc R H
H7B 1 0.3324(20) 0.1848(14) 0.3636(40) 0.056 Uiso calc R H
H7C 1 0.3147(26) 0.0624(54) 0.2754(10) 0.056 Uiso calc R H
C8 1 0.1864(6) 0.1210(11) 0.0846(6) 0.037(2) Uani d . C
H8A 1 0.1337(19) 0.1250(56) 0.0223(14) 0.055 Uiso calc R H
H8B 1 0.2024(43) 0.0200(19) 0.1029(18) 0.055 Uiso calc R H
H8C 1 0.2509(26) 0.1698(39) 0.0700(30) 0.055 Uiso calc R H
C9 1 -0.0204(7) 0.3119(10) 0.0616(6) 0.033(2) Uani d . C
H9A 1 -0.0775(27) 0.3777(49) 0.0739(8) 0.049 Uiso calc R H
H9B 1 -0.0503(37) 0.2224(12) 0.0299(22) 0.049 Uiso calc R H
H9C 1 0.0238(12) 0.3577(57) 0.0142(17) 0.049 Uiso calc R H
C10 1 -0.0708(6) 0.3903(9) 0.2980(6) 0.025(2) Uani d . C
H10A 1 -0.0544(6) 0.4768(9) 0.3423(6) 0.029 Uiso calc R H
H10B 1 -0.1171(6) 0.4201(9) 0.2341(6) 0.029 Uiso calc R H
C11 1 -0.1268(6) 0.2780(9) 0.3577(6) 0.025(2) Uani d . C
H11A 1 -0.1993(6) 0.3117(9) 0.3634(6) 0.030 Uiso calc R H
H11B 1 -0.0891(6) 0.2687(9) 0.4295(6) 0.030 Uiso calc R H
C12 1 -0.1700(6) 0.0261(9) 0.3788(6) 0.028(2) Uani d . C
H12A 1 -0.1731(39) -0.0697(13) 0.3463(18) 0.043 Uiso calc R H
H12B 1 -0.2405(18) 0.0538(32) 0.3938(32) 0.043 Uiso calc R H
H12C 1 -0.1214(23) 0.0238(41) 0.4441(17) 0.043 Uiso calc R H
C13 1 -0.2089(6) 0.1348(9) 0.2099(6) 0.026(2) Uani d . C
H13A 1 -0.2798(9) 0.1525(58) 0.2284(7) 0.039 Uiso calc R H
H13B 1 -0.2076(31) 0.0416(22) 0.1742(23) 0.039 Uiso calc R H
H13C 1 -0.1903(25) 0.2117(39) 0.1633(19) 0.039 Uiso calc R H
C14 1 -0.0262(6) -0.1958(8) 0.2121(5) 0.018(2) Uani d . C
C15 1 0.0336(6) -0.1982(10) 0.3276(6) 0.022(2) Uani d . C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 .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_publ_flag
O1 Rh1 C5 140.4(3) ?
O1 Rh1 C1 165.6(3) ?
C5 Rh1 C1 39.6(3) ?
O1 Rh1 O2 79.1(2) yes
C5 Rh1 O2 139.8(3) ?
C1 Rh1 O2 104.9(2) ?
O1 Rh1 C4 106.1(3) ?
C5 Rh1 C4 40.3(3) ?
C1 Rh1 C4 66.1(3) ?
O2 Rh1 C4 162.5(3) ?
O1 Rh1 C2 126.4(3) ?
C5 Rh1 C2 67.2(3) ?
C1 Rh1 C2 40.0(3) ?
O2 Rh1 C2 97.4(3) ?
C4 Rh1 C2 65.9(3) ?
O1 Rh1 N1 89.1(2) yes
C5 Rh1 N1 82.4(3) ?
C1 Rh1 N1 104.3(3) ?
O2 Rh1 N1 93.8(2) yes
C4 Rh1 N1 102.9(3) ?
C2 Rh1 N1 144.2(3) ?
O1 Rh1 C3 101.0(3) ?
C5 Rh1 C3 66.6(3) ?
C1 Rh1 C3 65.1(3) ?
O2 Rh1 C3 123.8(3) ?
C4 Rh1 C3 39.4(3) ?
C2 Rh1 C3 38.0(3) ?
N1 Rh1 C3 142.2(3) ?
C14 O1 Rh1 115.4(4) ?
C15 O2 Rh1 115.9(5) ?
C11 N1 C12 108.5(6) ?
C11 N1 C13 110.4(6) ?
C12 N1 C13 107.5(6) ?
C11 N1 Rh1 103.8(4) ?
C12 N1 Rh1 116.6(5) ?
C13 N1 Rh1 109.9(5) ?
C5 C1 C2 108.9(7) ?
C5 C1 C6 125.9(7) ?
C2 C1 C6 125.2(7) ?
C5 C1 Rh1 69.2(4) ?
C2 C1 Rh1 71.3(4) ?
C6 C1 Rh1 127.0(5) ?
C3 C2 C1 107.5(7) ?
C3 C2 C7 127.7(7) ?
C1 C2 C7 124.7(7) ?
C3 C2 Rh1 72.4(4) ?
C1 C2 Rh1 68.7(4) ?
C7 C2 Rh1 126.2(6) ?
C2 C3 C4 108.3(7) ?
C2 C3 C8 127.2(7) ?
C4 C3 C8 124.2(7) ?
C2 C3 Rh1 69.6(4) ?
C4 C3 Rh1 67.8(4) ?
C8 C3 Rh1 124.5(6) ?
C3 C4 C5 108.1(7) ?
C3 C4 C9 124.3(7) ?
C5 C4 C9 127.6(7) ?
C3 C4 Rh1 72.8(5) ?
C5 C4 Rh1 68.7(4) ?
C9 C4 Rh1 126.9(6) ?
C1 C5 C4 107.0(7) ?
C1 C5 C10 125.9(7) ?
C4 C5 C10 125.8(7) ?
C1 C5 Rh1 71.2(4) ?
C4 C5 Rh1 71.0(4) ?
C10 C5 Rh1 113.0(5) ?
C11 C10 C5 109.1(7) ?
C10 C11 N1 112.7(6) ?
O3 C14 C15 120.7(7) ?
O3 C14 O1 125.1(6) ?
C15 C14 O1 114.2(7) ?
O4 C15 O2 125.7(7) ?
O4 C15 C14 119.4(7) ?
O2 C15 C14 114.8(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Rh1 O1 2.089(5) y
Rh1 C5 2.092(7) y
Rh1 C1 2.119(8) y
Rh1 O2 2.081(5) y
Rh1 C4 2.123(8) y
Rh1 C2 2.154(8) y
Rh1 N1 2.188(6) y
Rh1 C3 2.191(8) y
O1 C14 1.294(9) ?
O2 C15 1.279(10) ?
O3 C14 1.211(9) ?
O4 C15 1.227(10) ?
N1 C11 1.496(9) ?
N1 C12 1.486(9) ?
N1 C13 1.480(9) ?
C1 C5 1.427(10) ?
C1 C2 1.461(11) ?
C1 C6 1.512(11) ?
C2 C3 1.414(11) ?
C2 C7 1.492(11) ?
C3 C4 1.455(11) ?
C3 C8 1.511(11) ?
C4 C5 1.452(11) ?
C4 C9 1.519(10) ?
C5 C10 1.503(11) ?
C10 C11 1.526(11) ?
C14 C15 1.583(9) ?
