#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/78/2227869.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_2227869
loop_
_publ_author_name
'Schmitt, Laurette'
'Labat, Gaël'
'Stoeckli-Evans, Helen'
_publ_section_title
;
 Aquachlorido(2,2':6',2''-terpyridyl)copper(II) chloride monohydrate
;
_journal_coeditor_code           OM2357
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1169
_journal_paper_doi               10.1107/S160053681003391X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu Cl (C15 H11 N3) (H2 O)] Cl, H2 O'
_chemical_formula_moiety         'C15 H13 Cl Cu N3 O, Cl H2 O'
_chemical_formula_sum            'C15 H15 Cl2 Cu N3 O2'
_chemical_formula_weight         403.74
_chemical_name_systematic
;
Aquachlorido(2,2':6',2''-terpyridyl)copper(II) chloride monohydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 107.532(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7155(8)
_cell_length_b                   13.6929(8)
_cell_length_c                   12.6599(10)
_cell_measurement_reflns_used    17467
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.69
_cell_volume                     1606.0(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2006)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2006)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2006)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '2-circle gonimometer'
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'phi + omega 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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14960
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULscanABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.699
_refine_ls_extinction_coef       0.0027(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2267
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0448P)²+1.3613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                2027
_reflns_number_total             2267
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om2357.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2227869
_cod_database_fobs_code          2227869
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,z
loop_
_atom_site_type_symbol
_atom_site_label
_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_occupancy
Cu Cu1 0.62103(3) 0.00000 0.15295(2) 0.02280(10) Uani . . 1.000
Cl Cl1 0.71809(7) 0.00000 0.01460(5) 0.0313(2) Uani . . 1.000
O O1W 0.8290(2) 0.00000 0.30520(15) 0.0297(5) Uani . . 1.000
N N1 0.5024(2) 0.00000 0.25225(16) 0.0220(5) Uani . . 1.000
N N2 0.59110(15) 0.14574(10) 0.16522(11) 0.0232(3) Uani . . 1.000
C C1 0.46408(17) -0.08528(12) 0.28568(13) 0.0236(4) Uani . . 1.000
C C2 0.38165(18) -0.08804(13) 0.35839(14) 0.0285(5) Uani . . 1.000
C C3 0.3403(3) 0.00000 0.3937(2) 0.0307(7) Uani . . 1.000
C C4 0.51479(17) 0.16973(12) 0.23508(13) 0.0232(4) Uani . . 1.000
C C5 0.48556(19) 0.26583(13) 0.25435(15) 0.0285(5) Uani . . 1.000
C C6 0.5360(2) 0.33929(13) 0.20053(16) 0.0324(5) Uani . . 1.000
C C7 0.6149(2) 0.31520(13) 0.12996(16) 0.0316(5) Uani . . 1.000
C C8 0.64036(19) 0.21726(13) 0.11436(14) 0.0281(5) Uani . . 1.000
Cl Cl2 0.1811(2) 0.17457(12) 0.53617(15) 0.0315(4) Uani . . 0.500
O O2W 0.1572(8) 0.1517(5) 0.5452(7) 0.0527(19) Uani . . 0.500
H H1 0.826(3) -0.0471(14) 0.3423(18) 0.0450 Uiso . . 1.000
H H2 0.35450 -0.14850 0.38310 0.0340 Uiso calc R 1.000
H H3 0.28300 0.00000 0.44270 0.0370 Uiso calc . 1.000
H H5 0.43180 0.28120 0.30370 0.0340 Uiso calc R 1.000
H H6 0.51640 0.40580 0.21210 0.0390 Uiso calc R 1.000
H H7 0.65110 0.36470 0.09280 0.0380 Uiso calc R 1.000
H H8 0.69460 0.20050 0.06590 0.0340 Uiso calc R 1.000
H H2A 0.070(2) 0.168(4) 0.520(6) 0.0790 Uiso . . 0.500
H H2B 0.215(5) 0.193(4) 0.534(7) 0.0790 Uiso . . 0.500
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'
Cu Cu 0.3201 1.2651 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Cu1 O1W . . . 100.56(5) no
Cl1 Cu1 N1 . . . 169.42(6) no
Cl1 Cu1 N2 . . . 99.48(4) no
Cl1 Cu1 N2 . . 4_555 99.48(4) no
O1W Cu1 N1 . . . 90.02(8) no
O1W Cu1 N2 . . . 92.59(4) no
O1W Cu1 N2 . . 4_555 92.59(4) no
N1 Cu1 N2 . . . 79.87(4) no
N1 Cu1 N2 . . 4_555 79.87(4) no
N2 Cu1 N2 . . 4_555 159.07(6) no
O2W Cl2 H2B . . . 163(10) no
H2A Cl2 H2B . . . 145(8) no
Cu1 O1W H1 . . 4_555 107.9(19) no
H1 O1W H1 . . 4_555 107(2) no
Cu1 O1W H1 . . . 107.9(19) no
H2A O2W H2B . . . 114(6) no
Cu1 N1 C1 . . 4_555 118.81(10) no
Cu1 N1 C1 . . . 118.81(10) no
C1 N1 C1 . . 4_555 122.37(18) no
C4 N2 C8 . . . 118.84(15) no
Cu1 N2 C8 . . . 127.08(12) no
Cu1 N2 C4 . . . 114.06(11) no
N1 C1 C4 . . 4_555 112.75(15) no
C2 C1 C4 . . 4_555 126.85(15) no
N1 C1 C2 . . . 120.37(16) no
C1 C2 C3 . . . 118.05(17) no
C2 C3 C2 . . 4_555 120.8(2) no
N2 C4 C1 . . 4_555 114.40(14) no
N2 C4 C5 . . . 121.85(15) no
C1 C4 C5 4_555 . . 123.74(16) no
C4 C5 C6 . . . 118.84(17) no
C5 C6 C7 . . . 119.51(17) no
C6 C7 C8 . . . 118.69(17) no
N2 C8 C7 . . . 122.27(17) no
C3 C2 H2 . . . 121.00 no
C1 C2 H2 . . . 121.00 no
C2 C3 H3 . . . 120.00 no
C2 C3 H3 4_555 . . 120.00 no
C4 C5 H5 . . . 121.00 no
C6 C5 H5 . . . 121.00 no
C7 C6 H6 . . . 120.00 no
C5 C6 H6 . . . 120.00 no
C6 C7 H7 . . . 121.00 no
C8 C7 H7 . . . 121.00 no
C7 C8 H8 . . . 119.00 no
N2 C8 H8 . . . 119.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 Cl1 . . 2.2253(7) no
Cu1 Cl1 . 2_655 3.3383(8) no
Cu1 O1W . . 2.3348(19) no
Cu1 N1 . . 1.945(2) no
Cu1 N2 . . 2.0294(14) no
Cu1 N2 . 4_555 2.0294(14) no
Cl2 O2W . . 0.426(8) no
Cl2 H2B . . 0.42(6) no
Cl2 H2A . . 1.04(3) no
O1W H1 . 4_555 0.80(2) no
O1W H1 . . 0.80(2) no
O2W H2B . . 0.84(6) no
O2W H2A . . 0.84(4) no
N1 C1 . . 1.3328(19) no
N1 C1 . 4_555 1.3328(19) no
N2 C8 . . 1.337(2) no
N2 C4 . . 1.355(2) no
C1 C4 . 4_555 1.477(2) no
C1 C2 . . 1.391(2) no
C2 C3 . . 1.387(2) no
C4 C5 . . 1.383(2) no
C5 C6 . . 1.385(3) no
C6 C7 . . 1.381(3) no
C7 C8 . . 1.389(3) no
C2 H2 . . 0.9500 no
C3 H3 . . 0.9500 no
C5 H5 . . 0.9500 no
C6 H6 . . 0.9500 no
C7 H7 . . 0.9500 no
C8 H8 . . 0.9500 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1 Cl2 3_656 0.80(2) 2.34(2) 3.143(2) 175(2) yes
O1W H1 O2W 3_656 0.80(2) 1.99(2) 2.787(8) 170(2) yes
O2W H2A O2W 2_556 0.84(2) 2.13(3) 2.922(15) 159(6) yes
C2 H2 Cl2 6_546 0.95 2.69 3.635(2) 172 yes
C5 H5 Cl2 7_556 0.95 2.65 3.593(3) 172 yes
C5 H5 O2W 7_556 0.95 2.50 3.429(8) 166 yes
C7 H7 Cl1 6_655 0.95 2.82 3.765(2) 175 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1W Cu1 N1 C1 . . . . -89.53(15) no
N2 Cu1 N1 C1 . . . . 177.85(17) no
N2 Cu1 N1 C1 . . . 4_555 -3.10(15) no
N2 Cu1 N1 C1 4_555 . . . 3.10(15) no
Cl1 Cu1 N2 C4 . . . . 171.96(11) no
Cl1 Cu1 N2 C8 . . . . -9.43(15) no
O1W Cu1 N2 C4 . . . . -86.88(12) no
O1W Cu1 N2 C8 . . . . 91.73(15) no
N1 Cu1 N2 C4 . . . . 2.68(12) no
N1 Cu1 N2 C8 . . . . -178.71(16) no
N2 Cu1 N2 C4 4_555 . . . 17.3(2) no
N2 Cu1 N2 C8 4_555 . . . -164.12(15) no
Cu1 N1 C1 C2 . . . . 178.75(13) no
Cu1 N1 C1 C4 . . . 4_555 -2.9(2) no
C1 N1 C1 C2 4_555 . . . -0.3(3) no
Cu1 N1 C1 C4 . . 4_555 . 2.9(2) no
C1 N1 C1 C4 . . 4_555 . -178.13(17) no
Cu1 N2 C4 C5 . . . . 179.30(13) no
Cu1 N2 C4 C1 . . . 4_555 -1.98(18) no
C8 N2 C4 C5 . . . . 0.6(2) no
C8 N2 C4 C1 . . . 4_555 179.29(15) no
Cu1 N2 C8 C7 . . . . -179.12(14) no
C4 N2 C8 C7 . . . . -0.6(3) no
N1 C1 C2 C3 . . . . 0.5(3) no
C4 C1 C2 C3 4_555 . . . -177.64(19) no
C2 C1 C4 N2 . . 4_555 4_555 178.71(16) no
C2 C1 C4 C5 . . 4_555 4_555 0.0(3) no
C1 C2 C3 C2 . . . 4_555 -0.8(3) no
N2 C4 C5 C6 . . . . 0.0(3) no
C1 C4 C5 C6 4_555 . . . -178.62(17) no
C4 C5 C6 C7 . . . . -0.5(3) no
C5 C6 C7 C8 . . . . 0.5(3) no
C6 C7 C8 N2 . . . . 0.0(3) no
