#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/09/2200939.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2200939
loop_
_publ_author_name
'Necefoglu, Hacali'
'Clegg, William'
'Scott, Andrew J.'
_publ_section_title
;
 A linear trinuclear CaZn₂ complex with bridging benzoate ligands
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m123
_journal_page_last               m124
_journal_paper_doi               10.1107/S160053680200209X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Ca Zn2 (C7 H5 O2)6 (C10 H14 N2 O)2]'
_chemical_formula_moiety         'C62 H58 Ca N4 O14 Zn2'
_chemical_formula_sum            'C62 H58 Ca N4 O14 Zn2'
_chemical_formula_weight         1253.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.207(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.347(2)
_cell_length_b                   10.7691(13)
_cell_length_c                   17.647(2)
_cell_measurement_reflns_used    7387
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.0
_cell_volume                     2967.6(6)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full .937
_diffrn_measured_fraction_theta_max .892
_diffrn_measurement_device_type  'Siemens SMART 1K CCD'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0394
_diffrn_reflns_av_sigmaI/netI    .0384
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12317
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .963
_exptl_absorpt_correction_T_max  .925
_exptl_absorpt_correction_T_min  .860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .16
_refine_diff_density_max         .407
_refine_diff_density_min         -.484
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          .0519
_refine_ls_R_factor_gt           .0398
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0348P)²+2.7427P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .0894
_refine_ls_wR_factor_ref         .0966
_reflns_number_gt                4193
_reflns_number_total             4938
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na6136.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2200939
_cod_database_fobs_code          2200939
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn .20197(2) .19710(3) .04078(2) .02835(11) Uani d . 1 . . Zn
Ca .0000 .0000 .0000 .02526(19) Uani d S 1 . . Ca
N1 .31448(15) .2969(2) .05654(15) .0326(6) Uani d . 1 . . N
C1 .3254(2) .4128(3) .0858(2) .0402(8) Uani d . 1 . . C
H1 .2846 .4472 .1087 .048 Uiso d R 1 . . H
C2 .4010(2) .4774(3) .0961(2) .0494(9) Uani d . 1 . . C
H2 .4008 .5642 .1054 .059 Uiso d R 1 . . H
C3 .4671(2) .4218(3) .0753(2) .0457(9) Uani d . 1 . . C
H3 .5205 .4637 .0862 .055 Uiso d R 1 . . H
C4 .45723(18) .3021(3) .04543(18) .0331(7) Uani d . 1 . . C
C5 .37961(18) .2441(3) .03646(18) .0326(7) Uani d . 1 . . C
H5 .3727 .1613 .0171 .039 Uiso d R 1 . . H
C6 .52377(18) .2415(3) .01435(18) .0329(7) Uani d . 1 . . C
O1 .52052(14) .2591(2) -.05501(13) .0457(6) Uani d . 1 . . O
N2 .58412(15) .1708(2) .06381(15) .0336(6) Uani d . 1 . . N
C7 .64967(18) .1126(3) .03345(19) .0368(7) Uani d . 1 . . C
H7A .6241 .0942 -.0237 .044 Uiso d R 1 . . H
H7B .6681 .0330 .0613 .044 Uiso d R 1 . . H
C8 .72458(19) .1991(3) .0403(2) .0421(8) Uani d . 1 . . C
H8A .7680 .1551 .0224 .063 Uiso d R 1 . . H
H8B .7484 .2208 .0965 .063 Uiso d R 1 . . H
H8C .7075 .2750 .0090 .063 Uiso d R 1 . . H
C9 .5898(2) .1471(3) .14682(18) .0415(8) Uani d . 1 . . C
H9A .5614 .2180 .1645 .050 Uiso d R 1 . . H
H9B .6505 .1459 .1796 .050 Uiso d R 1 . . H
C10 .5496(2) .0237(4) .1576(2) .0596(11) Uani d . 1 . . C
H10A .4962 .0128 .1146 .089 Uiso d R 1 . . H
H10B .5370 .0271 .2085 .089 Uiso d R 1 . . H
H10C .5880 -.0464 .1579 .089 Uiso d R 1 . . H
O2 .13990(12) .32848(19) .07535(12) .0331(5) Uani d . 1 . . O
O3 .02892(14) .2024(2) .03401(14) .0445(6) Uani d . 1 . . O
C11 .06069(19) .3030(3) .06260(17) .0305(7) Uani d . 1 . . C
C12 .00513(17) .3999(3) .08220(16) .0285(6) Uani d . 1 . . C
C13 .0394(2) .5109(3) .11757(19) .0364(7) Uani d . 1 . . C
H13 .0994 .5250 .1315 .044 Uiso d R 1 . . H
C14 -.0128(2) .5995(3) .1358(2) .0462(8) Uani d . 1 . . C
H14 .0083 .6770 .1593 .055 Uiso d R 1 . . H
C15 -.1001(2) .5788(3) .1178(2) .0454(9) Uani d . 1 . . C
H15 -.1370 .6380 .1307 .054 Uiso d R 1 . . H
C16 -.1344(2) .4694(3) .0823(2) .0429(8) Uani d . 1 . . C
H16 -.1947 .4582 .0672 .051 Uiso d R 1 . . H
C17 -.08257(19) .3798(3) .06443(18) .0371(7) Uani d . 1 . . C
H17 -.1057 .3010 .0450 .044 Uiso d R 1 . . H
O4 .18972(12) .14893(19) -.06907(12) .0352(5) Uani d . 1 . . O
O5 .07706(14) .0230(2) -.09016(13) .0449(6) Uani d . 1 . . O
C18 .13757(18) .0683(3) -.10940(17) .0306(7) Uani d . 1 . . C
C19 .15360(17) .0265(3) -.18477(17) .0292(6) Uani d . 1 . . C
C20 .11088(19) -.0769(3) -.22417(19) .0399(8) Uani d . 1 . . C
H20 .0714 -.1190 -.2031 .048 Uiso d R 1 . . H
C21 .1268(2) -.1202(3) -.2926(2) .0473(9) Uani d . 1 . . C
H21 .0957 -.1897 -.3197 .057 Uiso d R 1 . . H
C22 .1856(2) -.0579(4) -.3216(2) .0487(9) Uani d . 1 . . C
H22 .2004 -.0875 -.3665 .058 Uiso d R 1 . . H
C23 .2278(2) .0450(3) -.28328(19) .0453(8) Uani d . 1 . . C
H23 .2673 .0891 -.3034 .054 Uiso d R 1 . . H
C24 .21239(19) .0873(3) -.21453(18) .0369(7) Uani d . 1 . . C
H24 .2407 .1601 -.1895 .044 Uiso d R 1 . . H
O6 .25188(13) .0520(2) .10273(12) .0367(5) Uani d . 1 . . O
O7 .12999(13) -.0504(2) .09010(13) .0442(6) Uani d . 1 . . O
C25 .20928(18) -.0414(3) .11458(17) .0319(7) Uani d . 1 . . C
C26 .26071(18) -.1454(3) .16197(16) .0309(7) Uani d . 1 . . C
C27 .2201(2) -.2521(3) .17617(19) .0435(8) Uani d . 1 . . C
H27 .1595 -.2584 .1561 .052 Uiso d R 1 . . H
C28 .2677(2) -.3484(3) .2199(2) .0521(9) Uani d . 1 . . C
H28 .2403 -.4241 .2259 .063 Uiso d R 1 . . H
C29 .3555(2) -.3397(3) .24893(19) .0463(9) Uani d . 1 . . C
H29 .3871 -.4007 .2846 .056 Uiso d R 1 . . H
C30 .3963(2) -.2341(3) .23457(19) .0419(8) Uani d . 1 . . C
H30 .4571 -.2315 .2496 .050 Uiso d R 1 . . H
C31 .34922(18) -.1373(3) .19134(17) .0340(7) Uani d . 1 . . C
H31 .3776 -.0633 .1838 .041 Uiso d R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca .2262 .3064 '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_3
_geom_angle
_geom_angle_publ_flag
N1 Zn O2 . . 96.04(9) yes
N1 Zn O4 . . 95.55(9) yes
N1 Zn O6 . . 97.64(9) yes
O2 Zn O4 . . 126.44(9) yes
O2 Zn O6 . . 125.51(9) yes
O4 Zn O6 . . 104.28(9) yes
O3 Ca O3 . 3 180.00(12) .
O3 Ca O5 . . 88.06(8) yes
O3 Ca O5 3 3 88.06(8) ?
O3 Ca O5 . 3 91.94(8) ?
O3 Ca O5 3 . 91.94(8) ?
O3 Ca O7 . . 88.09(8) yes
O3 Ca O7 3 3 88.09(8) ?
O3 Ca O7 . 3 91.91(8) ?
O3 Ca O7 3 . 91.91(8) ?
O5 Ca O5 . 3 180.00(7) ?
O5 Ca O7 . . 85.49(8) yes
O5 Ca O7 3 3 85.49(8) ?
O5 Ca O7 3 . 94.51(8) ?
O5 Ca O7 . 3 94.51(8) ?
O7 Ca O7 . 3 180.00(18) ?
Zn N1 C1 . . 123.0(2) ?
Zn N1 C5 . . 119.0(2) ?
C1 N1 C5 . . 118.0(3) ?
N1 C1 C2 . . 122.0(3) ?
C1 C2 C3 . . 119.2(3) ?
C2 C3 C4 . . 119.6(3) ?
C3 C4 C5 . . 117.7(3) ?
C3 C4 C6 . . 121.8(3) ?
C5 C4 C6 . . 120.1(3) ?
N1 C5 C4 . . 123.5(3) ?
C4 C6 O1 . . 118.3(3) ?
C4 C6 N2 . . 118.7(3) ?
O1 C6 N2 . . 123.0(3) ?
C6 N2 C7 . . 118.6(3) ?
C6 N2 C9 . . 124.5(3) ?
C7 N2 C9 . . 117.0(2) ?
N2 C7 C8 . . 111.6(3) ?
N2 C9 C10 . . 112.1(3) ?
Zn O2 C11 . . 112.66(18) yes
Ca O3 C11 . . 166.6(2) yes
O2 C11 O3 . . 122.6(3) ?
O2 C11 C12 . . 117.7(3) ?
O3 C11 C12 . . 119.6(3) ?
C11 C12 C13 . . 121.0(3) ?
C11 C12 C17 . . 119.8(3) ?
C13 C12 C17 . . 119.2(3) ?
C12 C13 C14 . . 120.3(3) ?
C13 C14 C15 . . 120.1(3) ?
C14 C15 C16 . . 119.7(3) ?
C15 C16 C17 . . 120.6(3) ?
C12 C17 C16 . . 120.0(3) ?
Zn O4 C18 . . 126.02(19) yes
Ca O5 C18 . . 150.7(2) yes
O4 C18 O5 . . 124.9(3) ?
O4 C18 C19 . . 115.9(2) ?
O5 C18 C19 . . 119.2(3) ?
C18 C19 C20 . . 119.5(3) ?
C18 C19 C24 . . 121.1(3) ?
C20 C19 C24 . . 119.4(3) ?
C19 C20 C21 . . 120.6(3) ?
C20 C21 C22 . . 119.1(3) ?
C21 C22 C23 . . 120.7(3) ?
C22 C23 C24 . . 120.0(3) ?
C19 C24 C23 . . 120.1(3) ?
Zn O6 C25 . . 124.59(19) yes
Ca O7 C25 . . 150.8(2) yes
O6 C25 O7 . . 124.7(3) ?
O6 C25 C26 . . 115.9(2) ?
O7 C25 C26 . . 119.4(3) ?
C25 C26 C27 . . 120.1(3) ?
C25 C26 C31 . . 120.8(3) ?
C27 C26 C31 . . 119.1(3) ?
C26 C27 C28 . . 120.1(3) ?
C27 C28 C29 . . 120.5(3) ?
C28 C29 C30 . . 119.7(3) ?
C29 C30 C31 . . 120.2(3) ?
C26 C31 C30 . . 120.4(3) ?
N1 C1 H1 . . 119.7 ?
C2 C1 H1 . . 117.4 ?
C3 C2 H2 . . 121.1 ?
C1 C2 H2 . . 118.0 ?
C2 C3 H3 . . 119.1 ?
C4 C3 H3 . . 121.1 ?
N1 C5 H5 . . 118.2 ?
C4 C5 H5 . . 118.2 ?
N2 C7 H7A . . 108.8 ?
C8 C7 H7A . . 107.0 ?
N2 C7 H7B . . 109.5 ?
C8 C7 H7B . . 111.9 ?
H7A C7 H7B . . 107.9 ?
C7 C8 H8A . . 108.8 ?
C7 C8 H8B . . 107.3 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 112.3 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
N2 C9 H9A . . 106.6 ?
C10 C9 H9A . . 112.0 ?
N2 C9 H9B . . 110.0 ?
C10 C9 H9B . . 108.1 ?
H9A C9 H9B . . 107.9 ?
C9 C10 H10A . . 109.0 ?
C9 C10 H10B . . 107.3 ?
H10A C10 H10B . . 109.5 ?
C9 C10 H10C . . 112.0 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C14 C13 H13 . . 119.4 ?
C12 C13 H13 . . 120.2 ?
C13 C14 H14 . . 122.7 ?
C15 C14 H14 . . 117.2 ?
C16 C15 H15 . . 118.9 ?
C14 C15 H15 . . 121.4 ?
C15 C16 H16 . . 119.1 ?
C17 C16 H16 . . 120.3 ?
C16 C17 H17 . . 120.0 ?
C12 C17 H17 . . 119.6 ?
C19 C20 H20 . . 119.1 ?
C21 C20 H20 . . 120.2 ?
C22 C21 H21 . . 121.5 ?
C20 C21 H21 . . 119.4 ?
C23 C22 H22 . . 117.8 ?
C21 C22 H22 . . 121.3 ?
C22 C23 H23 . . 121.2 ?
C24 C23 H23 . . 118.8 ?
C23 C24 H24 . . 119.2 ?
C19 C24 H24 . . 120.7 ?
C28 C27 H27 . . 120.4 ?
C26 C27 H27 . . 119.6 ?
C29 C28 H28 . . 119.4 ?
C27 C28 H28 . . 119.9 ?
C28 C29 H29 . . 120.2 ?
C30 C29 H29 . . 119.6 ?
C29 C30 H30 . . 119.7 ?
C31 C30 H30 . . 119.8 ?
C30 C31 H31 . . 119.6 ?
C26 C31 H31 . . 119.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn N1 . 2.077(2) yes
Zn O2 . 1.942(2) yes
Zn O4 . 1.959(2) yes
Zn O6 . 1.943(2) yes
Ca O3 . 2.273(2) yes
Ca O3 3 2.273(2) .
Ca O5 . 2.316(2) yes
Ca O5 3 2.316(2) ?
Ca O7 . 2.311(2) yes
Ca O7 3 2.311(2) ?
N1 C1 . 1.342(4) ?
N1 C5 . 1.343(4) ?
C1 C2 . 1.382(4) ?
C2 C3 . 1.377(5) ?
C3 C4 . 1.384(4) ?
C4 C5 . 1.380(4) ?
C4 C6 . 1.505(4) ?
C6 O1 . 1.224(4) ?
C6 N2 . 1.344(4) ?
N2 C7 . 1.472(4) ?
N2 C9 . 1.463(4) ?
C7 C8 . 1.515(4) ?
C9 C10 . 1.519(5) ?
O2 C11 . 1.277(3) yes
O3 C11 . 1.242(3) yes
C11 C12 . 1.489(4) ?
C12 C13 . 1.388(4) ?
C12 C17 . 1.391(4) ?
C13 C14 . 1.380(4) ?
C14 C15 . 1.386(5) ?
C15 C16 . 1.374(5) ?
C16 C17 . 1.381(4) ?
O4 C18 . 1.276(3) yes
O5 C18 . 1.238(3) yes
C18 C19 . 1.499(4) ?
C19 C20 . 1.387(4) ?
C19 C24 . 1.388(4) ?
C20 C21 . 1.390(4) ?
C21 C22 . 1.388(5) ?
C22 C23 . 1.373(5) ?
C23 C24 . 1.387(4) ?
O6 C25 . 1.275(4) yes
O7 C25 . 1.243(3) yes
C25 C26 . 1.498(4) ?
C26 C27 . 1.387(4) ?
C26 C31 . 1.388(4) ?
C27 C28 . 1.386(5) ?
C28 C29 . 1.378(5) ?
C29 C30 . 1.379(5) ?
C30 C31 . 1.384(4) ?
C1 H1 . .950 ?
C2 H2 . .950 ?
C3 H3 . .950 ?
C5 H5 . .950 ?
C7 H7A . .990 ?
C7 H7B . .990 ?
C8 H8A . .980 ?
C8 H8B . .980 ?
C8 H8C . .980 ?
C9 H9A . .990 ?
C9 H9B . .990 ?
C10 H10A . .980 ?
C10 H10B . .980 ?
C10 H10C . .980 ?
C13 H13 . .950 ?
C14 H14 . .950 ?
C15 H15 . .950 ?
C16 H16 . .950 ?
C17 H17 . .950 ?
C20 H20 . .950 ?
C21 H21 . .950 ?
C22 H22 . .950 ?
C23 H23 . .950 ?
C24 H24 . .950 ?
C27 H27 . .950 ?
C28 H28 . .950 ?
C29 H29 . .950 ?
C30 H30 . .950 ?
C31 H31 . .950 ?
