#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:18:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179747 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/43/7004300.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_7004300
loop_
_publ_author_name
'Santillan, Guillermo A.'
'Carrano, Carl J.'
_publ_section_title
;
 Nickel(ii), copper(ii), and cobalt(ii) solid-state structures formed
 through hydrogen bonding with ditopic heteroscorpionate ligands
;
_journal_issue                   30
_journal_name_full               'Dalton Transactions'
_journal_page_first              3995
_journal_page_last               4005
_journal_paper_doi               10.1039/B805253K
_journal_year                    2008
_chemical_formula_sum            'C37 H38 Cu2 N8 O15 S2'
_chemical_formula_weight         1025.95
_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                90.931(6)
_cell_angle_beta                 107.725(6)
_cell_angle_gamma                107.444(6)
_cell_formula_units_Z            1
_cell_length_a                   9.8250(10)
_cell_length_b                   10.0588(10)
_cell_length_c                   11.9426(12)
_cell_measurement_reflns_used    2977
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.59
_cell_volume                     1065.00(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17185
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.7989
_exptl_absorpt_correction_T_min  0.7194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0941P)²+1.5241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                3256
_reflns_number_total             4701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B805253K.txt
_cod_data_source_block           gs68
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1064.99(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004300
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.58550(6) 0.63656(5) 0.87089(5) 0.0252(2) Uani 1 1 d . . .
N1 N 0.7496(4) 0.6184(4) 0.8169(3) 0.0222(8) Uani 1 1 d . . .
N2 N 0.8283(4) 0.7248(4) 0.7676(3) 0.0206(8) Uani 1 1 d . . .
N3 N 0.6739(4) 0.8434(4) 0.9017(3) 0.0193(8) Uani 1 1 d . . .
N4 N 0.7725(4) 0.9131(4) 0.8460(3) 0.0187(8) Uani 1 1 d . . .
S1 S 0.32552(13) 0.46200(12) 0.84410(11) 0.0257(3) Uani 1 1 d . . .
O1 O 0.1751(4) 0.9126(4) 0.4464(3) 0.0381(9) Uani 1 1 d . . .
O2 O 0.3227(4) 1.0202(4) 0.6252(3) 0.0341(8) Uani 1 1 d . . .
O3 O 0.3796(4) 0.6185(3) 0.8755(3) 0.0328(8) Uani 1 1 d . . .
O4 O 0.4570(4) 0.4389(3) 0.8196(3) 0.0330(8) Uani 1 1 d . . .
O5 O 0.2960(4) 0.3896(4) 0.9425(3) 0.0363(9) Uani 1 1 d . . .
O6 O 0.1935(4) 0.4182(4) 0.7393(3) 0.0404(9) Uani 1 1 d . . .
C1 C 1.0522(6) 0.7934(6) 0.6975(5) 0.0410(13) Uani 1 1 d . . .
H1A H 1.0208 0.8743 0.6788 0.061 Uiso 1 1 calc R . .
H1B H 1.0505 0.7457 0.6265 0.061 Uiso 1 1 calc R . .
H1C H 1.1527 0.8224 0.7529 0.061 Uiso 1 1 calc R . .
C2 C 0.9469(5) 0.6962(5) 0.7509(4) 0.0247(10) Uani 1 1 d . . .
C3 C 0.9453(6) 0.5696(5) 0.7915(4) 0.0294(11) Uani 1 1 d . . .
H3A H 1.0138 0.5225 0.7927 0.035 Uiso 1 1 calc R . .
C4 C 0.8219(6) 0.5252(5) 0.8307(4) 0.0252(10) Uani 1 1 d . . .
C5 C 0.7711(7) 0.3943(5) 0.8856(5) 0.0370(13) Uani 1 1 d . . .
H5B H 0.6816 0.3914 0.9037 0.055 Uiso 1 1 calc R . .
H5C H 0.8493 0.3938 0.9571 0.055 Uiso 1 1 calc R . .
H5D H 0.7500 0.3137 0.8312 0.055 Uiso 1 1 calc R . .
C6 C 0.9654(5) 1.1454(5) 0.8564(5) 0.0301(11) Uani 1 1 d . . .
H6B H 0.9748 1.0995 0.7893 0.045 Uiso 1 1 calc R . .
H6C H 1.0603 1.1732 0.9192 0.045 Uiso 1 1 calc R . .
H6D H 0.9366 1.2269 0.8343 0.045 Uiso 1 1 calc R . .
C7 C 0.8471(5) 1.0462(4) 0.8977(4) 0.0210(9) Uani 1 1 d . . .
C8 C 0.7951(5) 1.0631(4) 0.9884(4) 0.0249(10) Uani 1 1 d . . .
H8A H 0.8246 1.1445 1.0399 0.030 Uiso 1 1 calc R . .
C9 C 0.6879(5) 0.9341(4) 0.9897(4) 0.0224(9) Uani 1 1 d . . .
C10 C 0.6032(6) 0.8944(5) 1.0749(4) 0.0315(11) Uani 1 1 d . . .
H10A H 0.5375 0.7992 1.0524 0.047 Uiso 1 1 calc R . .
H10B H 0.5445 0.9556 1.0742 0.047 Uiso 1 1 calc R . .
H10C H 0.6731 0.9028 1.1530 0.047 Uiso 1 1 calc R . .
C11 C 0.7754(5) 0.8442(4) 0.7394(4) 0.0206(9) Uani 1 1 d . . .
H11A H 0.8490 0.9113 0.7107 0.025 Uiso 1 1 calc R . .
C12 C 0.6241(5) 0.8039(4) 0.6413(4) 0.0220(9) Uani 1 1 d . . .
C13 C 0.5242(5) 0.8766(4) 0.6372(4) 0.0217(9) Uani 1 1 d . . .
H13A H 0.5449 0.9445 0.6991 0.026 Uiso 1 1 calc R . .
C14 C 0.3929(5) 0.8491(4) 0.5410(4) 0.0230(10) Uani 1 1 d . . .
C15 C 0.2854(6) 0.9288(5) 0.5326(4) 0.0288(11) Uani 1 1 d . . .
C16 C 0.3628(6) 0.7452(6) 0.4499(5) 0.0390(13) Uani 1 1 d . . .
H16A H 0.2736 0.7235 0.3865 0.047 Uiso 1 1 calc R . .
C17 C 0.4634(7) 0.6745(6) 0.4527(5) 0.0466(15) Uani 1 1 d . . .
H17A H 0.4437 0.6075 0.3903 0.056 Uiso 1 1 calc R . .
C18 C 0.5930(6) 0.7031(5) 0.5478(4) 0.0327(12) Uani 1 1 d . . .
H18A H 0.6607 0.6546 0.5498 0.039 Uiso 1 1 calc R . .
O7 O 0.1381(4) 0.1607(4) 0.6148(4) 0.0521(11) Uani 1 1 d . . .
O8 O 1.0000 0.5000 0.5000 0.290(14) Uani 1 2 d S . .
C19 C 0.854(3) 0.546(2) 0.487(2) 0.113(8) Uani 0.50 1 d P . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 O4 95.26(15) . . ?
N1 Cu1 N3 92.39(15) . . ?
O4 Cu1 N3 167.44(15) . . ?
N1 Cu1 O3 161.52(16) . . ?
O4 Cu1 O3 71.50(14) . . ?
N3 Cu1 O3 98.67(14) . . ?
N1 Cu1 O5 92.38(15) . 2_667 ?
O4 Cu1 O5 97.45(14) . 2_667 ?
N3 Cu1 O5 92.16(14) . 2_667 ?
O3 Cu1 O5 101.89(15) . 2_667 ?
N1 Cu1 S1 130.42(11) . . ?
O4 Cu1 S1 35.63(10) . . ?
N3 Cu1 S1 134.65(11) . . ?
O3 Cu1 S1 36.06(10) . . ?
O5 Cu1 S1 99.11(9) 2_667 . ?
C4 N1 N2 105.5(4) . . ?
C4 N1 Cu1 132.5(3) . . ?
N2 N1 Cu1 121.4(3) . . ?
C2 N2 N1 110.8(4) . . ?
C2 N2 C11 130.0(4) . . ?
N1 N2 C11 119.2(4) . . ?
C9 N3 N4 106.1(3) . . ?
C9 N3 Cu1 131.7(3) . . ?
N4 N3 Cu1 120.0(3) . . ?
C7 N4 N3 111.2(3) . . ?
C7 N4 C11 129.2(4) . . ?
N3 N4 C11 119.3(3) . . ?
O6 S1 O5 110.9(2) . . ?
O6 S1 O4 110.6(2) . . ?
O5 S1 O4 111.0(2) . . ?
O6 S1 O3 111.2(2) . . ?
O5 S1 O3 111.2(2) . . ?
O4 S1 O3 101.7(2) . . ?
O6 S1 Cu1 129.14(17) . . ?
O5 S1 Cu1 119.96(16) . . ?
O4 S1 Cu1 50.67(13) . . ?
O3 S1 Cu1 51.35(14) . . ?
S1 O3 Cu1 92.59(17) . . ?
S1 O4 Cu1 93.70(17) . . ?
S1 O5 Cu1 140.8(2) . 2_667 ?
N2 C2 C3 106.3(4) . . ?
N2 C2 C1 122.5(4) . . ?
C3 C2 C1 131.1(4) . . ?
C2 C3 C4 106.8(4) . . ?
N1 C4 C3 110.5(4) . . ?
N1 C4 C5 121.2(4) . . ?
C3 C4 C5 128.2(5) . . ?
N4 C7 C8 106.5(4) . . ?
N4 C7 C6 122.5(4) . . ?
C8 C7 C6 131.0(4) . . ?
C7 C8 C9 107.0(4) . . ?
N3 C9 C8 109.2(4) . . ?
N3 C9 C10 122.1(4) . . ?
C8 C9 C10 128.7(4) . . ?
N2 C11 N4 109.8(3) . . ?
N2 C11 C12 112.3(3) . . ?
N4 C11 C12 112.3(4) . . ?
C13 C12 C18 119.5(4) . . ?
C13 C12 C11 120.6(4) . . ?
C18 C12 C11 119.5(4) . . ?
C12 C13 C14 120.5(4) . . ?
C13 C14 C16 118.8(5) . . ?
C13 C14 C15 121.6(4) . . ?
C16 C14 C15 119.6(4) . . ?
O1 C15 O2 123.1(5) . . ?
O1 C15 C14 122.7(5) . . ?
O2 C15 C14 114.1(4) . . ?
C17 C16 C14 120.8(5) . . ?
C16 C17 C18 119.8(5) . . ?
C17 C18 C12 120.6(5) . . ?
C19 O8 C19 180.0(18) . 2_766 ?
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
Cu1 N1 1.963(4) . ?
Cu1 O4 1.977(3) . ?
Cu1 N3 1.979(3) . ?
Cu1 O3 1.994(4) . ?
Cu1 O5 2.239(4) 2_667 ?
Cu1 S1 2.5505(13) . ?
N1 C4 1.321(6) . ?
N1 N2 1.375(5) . ?
N2 C2 1.350(6) . ?
N2 C11 1.451(5) . ?
N3 C9 1.326(6) . ?
N3 N4 1.369(5) . ?
N4 C7 1.349(5) . ?
N4 C11 1.452(5) . ?
S1 O6 1.447(4) . ?
S1 O5 1.451(4) . ?
S1 O4 1.489(4) . ?
S1 O3 1.503(3) . ?
O1 C15 1.213(6) . ?
O2 C15 1.312(6) . ?
O5 Cu1 2.239(4) 2_667 ?
C1 C2 1.500(7) . ?
C2 C3 1.367(7) . ?
C3 C4 1.384(7) . ?
C4 C5 1.499(6) . ?
C6 C7 1.503(6) . ?
C7 C8 1.359(7) . ?
C8 C9 1.409(6) . ?
C9 C10 1.489(7) . ?
C11 C12 1.520(6) . ?
C12 C13 1.379(6) . ?
C12 C18 1.392(6) . ?
C13 C14 1.391(6) . ?
C14 C16 1.395(7) . ?
C14 C15 1.487(7) . ?
C16 C17 1.372(8) . ?
C17 C18 1.373(7) . ?
O8 C19 1.60(3) . ?
O8 C19 1.60(3) 2_766 ?
