#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/72/1517291.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_1517291
loop_
_publ_author_name
'Jennifer, Samson Jegan'
'Muthiah, Packianathan Thomas'
_publ_section_title
;
 Synthesis, crystal structures and supramolecular architectures of square
 pyramidal Cu(II) complexes containing aromatic chelating N,N'-donor
 ligands
;
_journal_issue                   1
_journal_name_full               'Chemistry Central Journal'
_journal_page_first              42
_journal_paper_doi               10.1186/1752-153X-8-42
_journal_volume                  8
_journal_year                    2014
_chemical_formula_moiety         'C17 H12 Cl Cu N3 O8 S, H2 O '
_chemical_formula_sum            'C17 H14 Cl Cu N3 O9 S'
_chemical_formula_weight         535.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.336(2)
_cell_angle_beta                 96.851(2)
_cell_angle_gamma                107.630(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6712(3)
_cell_length_b                   10.3617(4)
_cell_length_c                   12.2860(4)
_cell_measurement_reflns_used    3540
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      1.7
_cell_volume                     1034.75(7)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18428
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_correction_T_min  0.9421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             542.0
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0331
_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)+(0.0468P)²+0.4213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                2974
_reflns_number_total             3540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2000794408128511_add3.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1034.75(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C17 H14 Cl Cu N3 O9 S '
_cod_database_code               1517291
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.20697(3) 0.24511(4) 0.73366(2) 0.04243(14) Uani 1 1 d .
S1 S 0.79149(9) 0.44428(8) 0.81828(6) 0.0517(2) Uani 1 1 d .
Cl1 Cl 1.15297(11) 0.54800(11) 0.87495(11) 0.0943(4) Uani 1 1 d .
C15 C -0.1632(3) 0.1381(3) 0.6791(2) 0.0451(7) Uani 1 1 d .
H15 H -0.1528 0.1471 0.6055 0.054 Uiso 1 1 calc R
C10 C 0.1019(3) 0.2000(3) 0.9391(2) 0.0353(6) Uani 1 1 d .
C9 C 0.0949(3) 0.1897(3) 1.0504(2) 0.0365(6) Uani 1 1 d .
C6 C 0.3839(3) 0.2830(3) 0.9679(2) 0.0492(7) Uani 1 1 d .
H6 H 0.4824 0.3148 0.9409 0.059 Uiso 1 1 calc R
C11 C -0.0450(3) 0.1605(3) 0.8608(2) 0.0352(6) Uani 1 1 d .
C12 C -0.1965(3) 0.1112(3) 0.8966(2) 0.0380(6) Uani 1 1 d .
C13 C -0.2010(3) 0.1026(3) 1.0110(2) 0.0434(7) Uani 1 1 d .
H13 H -0.3015 0.0710 1.0355 0.052 Uiso 1 1 calc R
C16 C -0.3178(3) 0.0886(3) 0.7057(2) 0.0467(7) Uani 1 1 d .
H16 H -0.4089 0.0648 0.6507 0.056 Uiso 1 1 calc R
C8 C 0.2470(3) 0.2298(3) 1.1232(2) 0.0426(6) Uani 1 1 d .
C1 C 0.5173(3) 0.3738(3) 0.6575(2) 0.0468(7) Uani 1 1 d .
C2 C 0.6968(3) 0.4350(3) 0.6855(2) 0.0464(7) Uani 1 1 d .
C14 C -0.0608(3) 0.1399(3) 1.0850(2) 0.0435(7) Uani 1 1 d .
H14 H -0.0665 0.1329 1.1594 0.052 Uiso 1 1 calc R
C17 C -0.3377(3) 0.0743(3) 0.8137(2) 0.0425(6) Uani 1 1 d .
C3 C 0.8090(4) 0.4847(3) 0.6186(3) 0.0600(9) Uani 1 1 d .
H3 H 0.7807 0.4875 0.5437 0.072 Uiso 1 1 calc R
C7 C 0.3888(3) 0.2761(3) 1.0799(2) 0.0489(7) Uani 1 1 d .
H7 H 0.4892 0.3030 1.1262 0.059 Uiso 1 1 calc R
C5 C 0.9789(4) 0.5131(3) 0.7792(3) 0.0624(9) Uani 1 1 d .
C4 C 0.9700(4) 0.5308(4) 0.6729(4) 0.0763(11) Uani 1 1 d .
H4 H 1.0604 0.5693 0.6391 0.092 Uiso 1 1 calc R
N2 N 0.2446(2) 0.2462(2) 0.89666(17) 0.0401(5) Uani 1 1 d .
N1 N -0.0269(2) 0.1739(2) 0.75380(17) 0.0402(5) Uani 1 1 d .
O1 O 0.4396(2) 0.3413(2) 0.73728(15) 0.0518(5) Uani 1 1 d .
O3 O 0.2399(3) 0.2183(2) 1.22957(15) 0.0546(5) Uani 1 1 d .
O2 O 0.4548(2) 0.3564(3) 0.55819(16) 0.0683(7) Uani 1 1 d .
O4 O -0.4824(2) 0.0275(3) 0.84763(18) 0.0607(6) Uani 1 1 d .
O1W O 0.1522(3) 0.2673(3) 0.57857(17) 0.0570(6) Uani 1 1 d .
O6 O 0.2654(2) 0.0332(2) 0.70787(18) 0.0610(6) Uani 1 1 d .
O2W O 0.5307(3) 0.3027(3) 0.35151(19) 0.0748(8) Uani 1 1 d .
N3 N 0.1872(3) -0.0627(3) 0.6321(2) 0.0514(6) Uani 1 1 d .
O7 O 0.0543(3) -0.0635(3) 0.5866(2) 0.0835(8) Uani 1 1 d .
O8 O 0.2451(4) -0.1510(3) 0.6036(2) 0.1023(10) Uani 1 1 d .
H1W H 0.230(6) 0.284(5) 0.554(4) 0.123 Uiso 1 1 d .
H3W H 0.516(6) 0.322(5) 0.408(4) 0.123 Uiso 1 1 d .
H2W H 0.092(6) 0.201(5) 0.534(4) 0.123 Uiso 1 1 d .
H4W H 0.573(6) 0.241(5) 0.360(4) 0.123 Uiso 1 1 d .
H4A H -0.543(6) 0.023(5) 0.801(4) 0.123 Uiso 1 1 d .
H5A H 0.347(6) 0.245(5) 1.272(4) 0.123 Uiso 1 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'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Cu1 O1W 92.61(8)
O1 Cu1 N2 90.24(8)
O1W Cu1 N2 170.36(10)
O1 Cu1 N1 169.15(9)
O1W Cu1 N1 93.31(9)
N2 Cu1 N1 82.50(8)
O1 Cu1 O6 88.53(8)
O1W Cu1 O6 99.53(9)
N2 Cu1 O6 89.73(8)
N1 Cu1 O6 99.44(9)
C5 S1 C2 90.44(16)
N1 C15 C16 123.2(2)
N2 C10 C9 124.0(2)
N2 C10 C11 115.7(2)
C9 C10 C11 120.3(2)
C10 C9 C14 119.0(2)
C10 C9 C8 117.0(2)
C14 C9 C8 124.0(2)
N2 C6 C7 123.0(2)
N1 C11 C12 123.9(2)
N1 C11 C10 116.4(2)
C12 C11 C10 119.7(2)
C11 C12 C13 119.1(2)
C11 C12 C17 116.5(2)
C13 C12 C17 124.4(2)
C14 C13 C12 120.9(2)
C15 C16 C17 119.9(2)
O3 C8 C7 124.6(2)
O3 C8 C9 116.8(2)
C7 C8 C9 118.5(2)
O2 C1 O1 125.5(3)
O2 C1 C2 117.9(2)
O1 C1 C2 116.6(2)
C3 C2 C1 129.3(3)
C3 C2 S1 110.7(2)
C1 C2 S1 119.9(2)
C13 C14 C9 121.0(2)
O4 C17 C16 124.3(2)
O4 C17 C12 116.6(2)
C16 C17 C12 119.1(2)
C2 C3 C4 113.7(3)
C8 C7 C6 120.5(2)
C4 C5 S1 113.3(2)
C4 C5 Cl1 127.4(3)
S1 C5 Cl1 119.2(2)
C5 C4 C3 111.8(3)
C6 N2 C10 117.0(2)
C6 N2 Cu1 130.29(18)
C10 N2 Cu1 112.68(16)
C15 N1 C11 117.4(2)
C15 N1 Cu1 129.94(18)
C11 N1 Cu1 112.67(16)
C1 O1 Cu1 129.13(18)
N3 O6 Cu1 123.01(17)
O8 N3 O7 120.8(3)
O8 N3 O6 120.4(3)
O7 N3 O6 118.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu1 O1 1.9538(18)
Cu1 O1W 1.960(2)
Cu1 N2 1.989(2)
Cu1 N1 1.991(2)
Cu1 O6 2.400(2)
S1 C5 1.711(3)
S1 C2 1.717(3)
Cl1 C5 1.720(3)
C15 N1 1.338(3)
C15 C16 1.373(4)
C10 N2 1.368(3)
C10 C9 1.389(3)
C10 C11 1.426(3)
C9 C14 1.423(4)
C9 C8 1.425(4)
C6 N2 1.333(3)
C6 C7 1.381(4)
C11 N1 1.357(3)
C11 C12 1.397(3)
C12 C13 1.421(4)
C12 C17 1.424(4)
C13 C14 1.357(4)
C16 C17 1.374(4)
C8 O3 1.330(3)
C8 C7 1.368(4)
C1 O2 1.248(3)
C1 O1 1.269(3)
C1 C2 1.475(4)
C2 C3 1.361(4)
C17 O4 1.333(3)
C3 C4 1.392(5)
C5 C4 1.331(5)
O6 N3 1.258(3)
N3 O8 1.214(3)
N3 O7 1.217(3)
