#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:43:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179489 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/86/4338693.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_4338693
loop_
_publ_author_name
'Santillan, Guillermo A.'
'Carrano, Carl J.'
_publ_section_title
;
 Cobalt, zinc, and nickel complexes of a diatopic heteroscorpionate
 ligand: building blocks for coordination polymers.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              930
_journal_page_last               939
_journal_paper_doi               10.1021/ic701718b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C36 H42 Cl2 N8 O14 Zn2'
_chemical_formula_weight         1012.46
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.027(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.0732(8)
_cell_length_b                   23.533(2)
_cell_length_c                   10.0066(9)
_cell_measurement_reflns_used    8084
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.76
_cell_volume                     2089.7(3)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41896
_diffrn_reflns_theta_full        34.80
_diffrn_reflns_theta_max         34.80
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.7737
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1675P)²+0.8264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2419
_refine_ls_wR_factor_ref         0.2617
_reflns_number_gt                6028
_reflns_number_total             9034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701718b-complex_7.cif
_cod_data_source_block           justin88
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4338693
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Zn1 Zn 0.44065(4) 0.401251(14) 0.82617(3) 0.03405(13) Uani 1 1 d .
N1 N 0.4225(3) 0.31952(10) 0.7475(3) 0.0338(5) Uani 1 1 d .
N2 N 0.2979(3) 0.30529(9) 0.6503(2) 0.0318(4) Uani 1 1 d .
N3 N 0.2136(3) 0.40795(10) 0.7941(2) 0.0289(4) Uani 1 1 d .
N4 N 0.1260(2) 0.37515(10) 0.6963(2) 0.0275(4) Uani 1 1 d .
O1 O 0.4666(3) 0.50721(11) 0.8150(2) 0.0436(5) Uani 1 1 d .
O2 O 0.5799(3) 0.43788(10) 0.7268(3) 0.0430(5) Uani 1 1 d .
O3 O 0.5308(3) 0.40044(10) 1.0244(3) 0.0436(5) Uani 1 1 d D
C1 C 0.1849(6) 0.22325(18) 0.5061(5) 0.0680(13) Uani 1 1 d .
H1A H 0.1067 0.2503 0.4729 0.102 Uiso 1 1 calc R
H1B H 0.1431 0.1913 0.5449 0.102 Uiso 1 1 calc R
H1C H 0.2288 0.2107 0.4318 0.102 Uiso 1 1 calc R
C2 C 0.3025(5) 0.25026(12) 0.6120(4) 0.0430(7) Uani 1 1 d .
C3 C 0.4347(6) 0.22853(14) 0.6883(4) 0.0538(9) Uani 1 1 d .
H3B H 0.4704 0.1916 0.6848 0.065 Uiso 1 1 calc R
C4 C 0.5046(4) 0.27227(14) 0.7715(3) 0.0443(7) Uani 1 1 d .
C5 C 0.6471(6) 0.2708(2) 0.8743(5) 0.0657(12) Uani 1 1 d .
H5A H 0.6667 0.3076 0.9152 0.099 Uiso 1 1 calc R
H5B H 0.7281 0.2603 0.8309 0.099 Uiso 1 1 calc R
H5C H 0.6393 0.2434 0.9435 0.099 Uiso 1 1 calc R
C6 C -0.1425(4) 0.3424(2) 0.6208(4) 0.0557(10) Uani 1 1 d .
H6A H -0.1026 0.3227 0.5522 0.084 Uiso 1 1 calc R
H6B H -0.2208 0.3679 0.5776 0.084 Uiso 1 1 calc R
H6C H -0.1832 0.3154 0.6753 0.084 Uiso 1 1 calc R
C7 C -0.0190(3) 0.37573(13) 0.7105(3) 0.0326(5) Uani 1 1 d .
C8 C -0.0244(4) 0.41018(15) 0.8207(3) 0.0396(6) Uani 1 1 d .
H8A H -0.1091 0.4189 0.8555 0.048 Uiso 1 1 calc R
C9 C 0.1229(3) 0.42941(12) 0.8700(3) 0.0331(5) Uani 1 1 d .
C10 C 0.1829(4) 0.4682(2) 0.9871(4) 0.0548(10) Uani 1 1 d .
H10A H 0.2894 0.4732 0.9947 0.082 Uiso 1 1 calc R
H10B H 0.1647 0.4519 1.0701 0.082 Uiso 1 1 calc R
H10C H 0.1333 0.5044 0.9718 0.082 Uiso 1 1 calc R
C11 C 0.1920(3) 0.34920(11) 0.5910(3) 0.0289(5) Uani 1 1 d .
H11A H 0.1104 0.3307 0.5259 0.035 Uiso 1 1 calc R
C12 C 0.2642(3) 0.39253(11) 0.5121(3) 0.0275(4) Uani 1 1 d .
C13 C 0.3788(4) 0.37564(12) 0.4466(3) 0.0384(6) Uani 1 1 d .
H13A H 0.4155 0.3387 0.4574 0.046 Uiso 1 1 calc R
C14 C 0.7278(4) 0.51396(13) 0.5833(3) 0.0363(6) Uani 1 1 d D
H14A H 0.775(6) 0.4796(13) 0.621(5) 0.071(16) Uiso 1 1 d D
C15 C 0.6156(3) 0.53101(12) 0.6499(3) 0.0298(5) Uani 1 1 d .
C16 C 0.4385(4) 0.41364(13) 0.3653(3) 0.0376(6) Uani 1 1 d D
H16A H 0.523(3) 0.4075(16) 0.324(4) 0.033(10) Uiso 1 1 d D
C17 C 0.2124(3) 0.44812(13) 0.4976(3) 0.0358(5) Uani 1 1 d D
H17A H 0.128(3) 0.4571(16) 0.536(3) 0.031(9) Uiso 1 1 d D
C18 C 0.5491(3) 0.49044(13) 0.7370(3) 0.0323(5) Uani 1 1 d .
Cl1 Cl 0.89672(13) 0.36106(6) 1.22248(12) 0.0696(3) Uani 1 1 d D
O7 O 0.9787(7) 0.3180(3) 1.2909(6) 0.131(2) Uani 1 1 d D
O6 O 0.7541(10) 0.3442(4) 1.1772(15) 0.318(9) Uani 1 1 d D
O5 O 0.8878(15) 0.4011(5) 1.3189(9) 0.227(6) Uani 1 1 d D
O4 O 0.944(2) 0.3843(5) 1.1283(14) 0.390(15) Uani 1 1 d D
H101 H 0.620(2) 0.3847(18) 1.052(4) 0.037(10) Uiso 1 1 d D
H100 H 0.613(4) 0.418(2) 1.069(5) 0.066(16) Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O2 Zn1 O3 109.66(12) . .
O2 Zn1 N3 128.81(10) . .
O3 Zn1 N3 110.70(11) . .
O2 Zn1 N1 102.92(11) . .
O3 Zn1 N1 110.80(10) . .
N3 Zn1 N1 90.83(10) . .
O2 Zn1 C18 29.22(10) . .
O3 Zn1 C18 104.40(10) . .
N3 Zn1 C18 109.50(9) . .
N1 Zn1 C18 129.44(10) . .
C4 N1 N2 105.8(3) . .
C4 N1 Zn1 135.2(2) . .
N2 N1 Zn1 119.01(17) . .
C2 N2 N1 111.4(3) . .
C2 N2 C11 128.5(3) . .
N1 N2 C11 119.6(2) . .
C9 N3 N4 106.7(2) . .
C9 N3 Zn1 132.03(19) . .
N4 N3 Zn1 119.43(17) . .
C7 N4 N3 110.7(2) . .
C7 N4 C11 129.6(2) . .
N3 N4 C11 119.5(2) . .
C18 O2 Zn1 102.16(19) . .
N2 C2 C3 105.8(3) . .
N2 C2 C1 123.6(4) . .
C3 C2 C1 130.6(3) . .
C2 C3 C4 107.0(3) . .
N1 C4 C3 110.0(3) . .
N1 C4 C5 121.5(4) . .
C3 C4 C5 128.6(4) . .
N4 C7 C8 106.7(2) . .
N4 C7 C6 123.6(3) . .
C8 C7 C6 129.7(3) . .
C7 C8 C9 106.4(3) . .
N3 C9 C8 109.6(2) . .
N3 C9 C10 120.7(3) . .
C8 C9 C10 129.7(3) . .
N2 C11 N4 109.9(2) . .
N2 C11 C12 111.7(2) . .
N4 C11 C12 112.5(2) . .
C17 C12 C13 119.2(3) . .
C17 C12 C11 120.9(2) . .
C13 C12 C11 119.8(2) . .
C16 C13 C12 120.6(3) . .
C15 C14 C17 120.6(3) . 3_666
C14 C15 C16 119.8(3) . 3_666
C14 C15 C18 121.3(3) . .
C16 C15 C18 119.0(3) 3_666 .
C13 C16 C15 119.6(3) . 3_666
C14 C17 C12 120.1(3) 3_666 .
O1 C18 O2 121.6(3) . .
O1 C18 C15 121.7(3) . .
O2 C18 C15 116.7(3) . .
O1 C18 Zn1 73.60(17) . .
O2 C18 Zn1 48.62(14) . .
C15 C18 Zn1 162.8(2) . .
O4 Cl1 O7 118.1(8) . .
O4 Cl1 O5 108.3(8) . .
O7 Cl1 O5 105.5(5) . .
O4 Cl1 O6 109.8(10) . .
O7 Cl1 O6 109.8(5) . .
O5 Cl1 O6 104.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.962(2) .
Zn1 O3 1.982(2) .
Zn1 N3 2.024(2) .
Zn1 N1 2.072(2) .
Zn1 C18 2.557(3) .
N1 C4 1.332(4) .
N1 N2 1.370(4) .
N2 C2 1.354(3) .
N2 C11 1.451(4) .
N3 C9 1.330(3) .
N3 N4 1.364(3) .
N4 C7 1.353(3) .
N4 C11 1.451(3) .
O1 C18 1.253(4) .
O2 C18 1.277(4) .
C1 C2 1.481(6) .
C2 C3 1.379(6) .
C3 C4 1.391(6) .
C4 C5 1.475(6) .
C6 C7 1.502(4) .
C7 C8 1.378(4) .
C8 C9 1.400(4) .
C9 C10 1.496(4) .
C11 C12 1.519(4) .
C12 C17 1.387(4) .
C12 C13 1.397(4) .
C13 C16 1.392(4) .
C14 C15 1.387(4) .
C14 C17 1.389(4) 3_666
C15 C16 1.389(4) 3_666
C15 C18 1.501(4) .
C16 C15 1.389(4) 3_666
C17 C14 1.389(4) 3_666
Cl1 O4 1.242(7) .
Cl1 O7 1.356(5) .
Cl1 O5 1.363(8) .
Cl1 O6 1.339(7) .
