#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:19:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179322 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/19/4321967.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_4321967
loop_
_publ_author_name
'Heather D. Hansen'
'Kalyani Maitra'
'John H. Nelson'
_publ_section_title
;
 Chloride Substitution Reactions of Cycloruthenated
 (R)C-(+)-N,N-Dimethyl(1-phenylethyl)amine with Pseudohalides: Ruthenium
 Atom Stereochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2150
_journal_page_last               2156
_journal_paper_doi               10.1021/ic981304d
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C17 H23 N2 O3 Ru'
_chemical_formula_weight         404.44
_chemical_name_common            3a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 92.250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.303
_cell_length_b                   14.3370(10)
_cell_length_c                   8.1670(10)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.25
_cell_measurement_theta_min      2.78
_cell_volume                     854.45(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2433
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.50
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.9375
_exptl_absorpt_correction_T_min  0.8185
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_size_max          .28
_exptl_crystal_size_mid          .66
_exptl_crystal_size_min          .36
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       0.0103(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   1.016
_refine_ls_goodness_of_fit_obs   1.018
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1694
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.018
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_obs          0.0184
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0276P)²+0.3276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0470
_refine_ls_wR_factor_obs         0.0462
_reflns_number_observed          1668
_reflns_number_total             1705
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981304d_2.cif
_cod_data_source_block           jhn018b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.3276P] 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^)+(0.0276P)^2^+0.3276P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.30599(3) 0.71962(3) 0.52632(3) 0.02711(10) Uani 1 d . .
N1 N 0.2086(4) 0.8224(2) 0.3471(4) 0.0326(7) Uani 1 d . .
N2 N 0.5037(5) 0.8137(3) 0.6163(4) 0.0390(8) Uani 1 d . .
O1 O 0.4609(6) 0.8886(3) 0.6740(6) 0.088(2) Uani 1 d . .
O2 O 0.6613(5) 0.7925(4) 0.6379(7) 0.120(2) Uani 1 d . .
C1 C 0.4817(5) 0.6990(2) 0.3372(4) 0.0294(11) Uani 1 d . .
C2 C 0.5914(5) 0.6210(3) 0.3136(5) 0.0413(9) Uani 1 d . .
H2A H 0.5936(5) 0.5735(3) 0.3911(5) 0.050 Uiso 1 calc R .
C3 C 0.6979(6) 0.6125(4) 0.1762(6) 0.0512(12) Uani 1 d . .
H3A H 0.7688(6) 0.5594(4) 0.1619(6) 0.061 Uiso 1 calc R .
C4 C 0.6975(6) 0.6830(4) 0.0621(6) 0.0567(15) Uani 1 d . .
H4A H 0.7676(6) 0.6773(4) -0.0300(6) 0.068 Uiso 1 calc R .
C5 C 0.5934(6) 0.7626(4) 0.0833(5) 0.0478(11) Uani 1 d . .
H5A H 0.5951(6) 0.8104(4) 0.0065(5) 0.057 Uiso 1 calc R .
C6 C 0.4846(5) 0.7708(3) 0.2220(4) 0.0337(8) Uani 1 d . .
C7 C 0.3726(6) 0.8558(3) 0.2558(5) 0.0375(9) Uani 1 d . .
H7A H 0.4462(6) 0.8942(3) 0.3327(5) 0.045 Uiso 1 calc R .
C8 C 0.3242(8) 0.9179(4) 0.1066(6) 0.0574(13) Uani 1 d . .
H8A H 0.2528(8) 0.9702(4) 0.1406(6) 0.086 Uiso 1 calc R .
H8B H 0.2547(8) 0.8824(4) 0.0262(6) 0.086 Uiso 1 calc R .
H8C H 0.4348(8) 0.9399(4) 0.0599(6) 0.086 Uiso 1 calc R .
C9 C 0.1164(7) 0.9020(3) 0.4282(6) 0.0523(12) Uani 1 d . .
H9A H 0.2013(7) 0.9314(3) 0.5048(6) 0.078 Uiso 1 calc R .
H9B H 0.0129(7) 0.8794(3) 0.4851(6) 0.078 Uiso 1 calc R .
H9C H 0.0759(7) 0.9466(3) 0.3468(6) 0.078 Uiso 1 calc R .
C10 C 0.0720(6) 0.7794(3) 0.2300(5) 0.0449(10) Uani 1 d . .
H10A H 0.1272(6) 0.7278(3) 0.1757(5) 0.067 Uiso 1 calc R .
H10B H 0.0319(6) 0.8250(3) 0.1503(5) 0.067 Uiso 1 calc R .
H10C H -0.0312(6) 0.7578(3) 0.2886(5) 0.067 Uiso 1 calc R .
C11 C 0.2683(8) 0.5690(3) 0.5500(7) 0.0570(14) Uani 1 d . .
H11A H 0.3316(8) 0.5267(3) 0.4767(7) 0.068 Uiso 1 calc R .
C12 C 0.0989(6) 0.6060(3) 0.5001(5) 0.0488(11) Uani 1 d . .
H12A H 0.0461(6) 0.5906(3) 0.3913(5) 0.059 Uiso 1 calc R .
C13 C 0.0213(6) 0.6768(4) 0.5910(6) 0.0514(11) Uani 1 d . .
H13A H -0.0832(6) 0.7113(4) 0.5424(6) 0.062 Uiso 1 calc R .
C14 C 0.1050(6) 0.7102(6) 0.7355(5) 0.0578(14) Uani 1 d . .
H14A H 0.0599(6) 0.7670(6) 0.7868(5) 0.069 Uiso 1 calc R .
C15 C 0.2776(8) 0.6744(4) 0.7818(5) 0.0606(14) Uani 1 d . .
H15A H 0.3500(8) 0.7061(4) 0.8687(5) 0.073 Uiso 1 calc R .
C16 C 0.3604(7) 0.6018(4) 0.6928(7) 0.0607(14) Uani 1 d . .
H16A H 0.4864(7) 0.5822(4) 0.7204(7) 0.073 Uiso 1 calc R .
C17 C 0.8202(7) 0.9957(4) 0.9250(7) 0.0610(13) Uani 1 d . .
H17A H 0.8011(7) 0.9676(4) 1.0297(7) 0.092 Uiso 1 calc R .
H17B H 0.7061(7) 1.0198(4) 0.8805(7) 0.092 Uiso 1 calc R .
H17C H 0.9071(7) 1.0457(4) 0.9380(7) 0.092 Uiso 1 calc R .
O3 O 0.8867(5) 0.9298(3) 0.8200(5) 0.0791(12) Uani 1 d . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables    4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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 Ru1 N2 85.07(13) . . ?
C1 Ru1 N1 77.91(12) . . ?
N2 Ru1 N1 90.15(13) . . ?
C1 Ru1 C11 90.5(2) . . ?
N2 Ru1 C11 134.0(2) . . ?
N1 Ru1 C11 133.6(2) . . ?
C1 Ru1 C16 104.5(2) . . ?
N2 Ru1 C16 100.0(2) . . ?
N1 Ru1 C16 169.7(2) . . ?
C11 Ru1 C16 37.4(2) . . ?
C1 Ru1 C15 138.6(2) . . ?
N2 Ru1 C15 86.9(2) . . ?
N1 Ru1 C15 142.7(2) . . ?
C11 Ru1 C15 67.0(2) . . ?
C16 Ru1 C15 37.6(2) . . ?
C1 Ru1 C12 105.24(15) . . ?
N2 Ru1 C12 164.50(14) . . ?
N1 Ru1 C12 103.19(15) . . ?
C11 Ru1 C12 36.7(2) . . ?
C16 Ru1 C12 66.6(2) . . ?
C15 Ru1 C12 77.7(2) . . ?
C1 Ru1 C13 138.0(2) . . ?
N2 Ru1 C13 136.6(2) . . ?
N1 Ru1 C13 93.55(15) . . ?
C11 Ru1 C13 65.7(2) . . ?
C16 Ru1 C13 77.9(2) . . ?
C15 Ru1 C13 64.9(2) . . ?
C12 Ru1 C13 36.2(2) . . ?
C1 Ru1 C14 168.4(3) . . ?
N2 Ru1 C14 103.3(2) . . ?
N1 Ru1 C14 109.8(2) . . ?
C11 Ru1 C14 77.9(3) . . ?
C16 Ru1 C14 66.4(3) . . ?
C15 Ru1 C14 36.1(2) . . ?
C12 Ru1 C14 65.0(2) . . ?
C13 Ru1 C14 35.6(2) . . ?
C10 N1 C9 107.4(3) . . ?
C10 N1 C7 109.7(3) . . ?
C9 N1 C7 110.9(3) . . ?
C10 N1 Ru1 110.2(2) . . ?
C9 N1 Ru1 111.1(3) . . ?
C7 N1 Ru1 107.5(2) . . ?
O2 N2 O1 115.3(4) . . ?
O2 N2 Ru1 122.4(4) . . ?
O1 N2 Ru1 121.4(3) . . ?
C2 C1 C6 118.3(3) . . ?
C2 C1 Ru1 126.5(3) . . ?
C6 C1 Ru1 115.1(3) . . ?
C1 C2 C3 121.6(4) . . ?
C4 C3 C2 119.6(4) . . ?
C3 C4 C5 120.5(4) . . ?
C4 C5 C6 119.8(5) . . ?
C1 C6 C5 120.2(4) . . ?
C1 C6 C7 116.9(3) . . ?
C5 C6 C7 122.9(4) . . ?
C6 C7 N1 106.4(3) . . ?
C6 C7 C8 115.8(4) . . ?
N1 C7 C8 114.3(3) . . ?
C12 C11 C16 120.4(5) . . ?
C12 C11 Ru1 73.2(3) . . ?
C16 C11 Ru1 71.6(3) . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 Ru1 72.8(3) . . ?
C11 C12 Ru1 70.0(3) . . ?
C12 C13 C14 121.9(5) . . ?
C12 C13 Ru1 71.0(2) . . ?
C14 C13 Ru1 74.1(2) . . ?
C13 C14 C15 117.7(6) . . ?
C13 C14 Ru1 70.3(2) . . ?
C15 C14 Ru1 68.2(2) . . ?
C14 C15 C16 121.9(5) . . ?
C14 C15 Ru1 75.7(3) . . ?
C16 C15 Ru1 70.9(3) . . ?
C11 C16 C15 118.1(5) . . ?
C11 C16 Ru1 71.0(3) . . ?
C15 C16 Ru1 71.5(3) . . ?
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
Ru1 C1 2.068(3) . ?
Ru1 N2 2.088(3) . ?
Ru1 N1 2.177(3) . ?
Ru1 C11 2.187(5) . ?
Ru1 C16 2.195(5) . ?
Ru1 C15 2.202(4) . ?
Ru1 C12 2.228(4) . ?
Ru1 C13 2.250(4) . ?
Ru1 C14 2.299(4) . ?
N1 C10 1.488(5) . ?
N1 C9 1.493(5) . ?
N1 C7 1.514(5) . ?
N2 O2 1.197(5) . ?
N2 O1 1.219(5) . ?
C1 C2 1.394(5) . ?
C1 C6 1.395(5) . ?
C2 C3 1.395(6) . ?
C3 C4 1.375(7) . ?
C4 C5 1.385(7) . ?
C5 C6 1.413(5) . ?
C6 C7 1.499(6) . ?
C7 C8 1.539(6) . ?
C11 C12 1.392(7) . ?
C11 C16 1.405(8) . ?
C12 C13 1.392(7) . ?
C13 C14 1.392(7) . ?
C14 C15 1.398(7) . ?
C15 C16 1.418(8) . ?
C17 O3 1.377(7) . ?
