#------------------------------------------------------------------------------
#$Date: 2017-07-25 12:01:08 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199071 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/07/2020778.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_2020778
loop_
_publ_author_name
'Guo, Pei-Ying'
'Ma, De-Yun'
'Guo, Hai-Fu'
_publ_section_title
;
 A twofold interpenetrating three-dimensional heterometallic
 metal--organic framework with pcu topology based on
 2-methylbiphenyl-4,4'-dicarboxylic acid
;
_journal_coeditor_code           FN3233
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              470
_journal_page_last               475
_journal_paper_doi               10.1107/S2053229617006829
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ca Zn6 (C15 H10 O4)6 (O H)2 (H2 O)3]'
_chemical_formula_moiety         'C90 H68 Ca O29 Zn6'
_chemical_formula_sum            'C90 H68 Ca O29 Zn6'
_chemical_formula_weight         2045.74
_chemical_name_systematic
Poly[triaquadi-μ₃-hydroxido-hexakis(μ₄-2-methylbiphenyl-4,4'-dicarboxylato)calcium(II)hexazinc(II)]
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.1506(12)
_cell_length_b                   33.1506(12)
_cell_length_c                   16.6829(14)
_cell_measurement_reflns_used    2704
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.07
_cell_measurement_theta_min      2.21
_cell_volume                     18333.9(18)
_computing_cell_refinement       SMART
_computing_data_collection
;
SMART (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al.,  2009) and
DIAMOND (Brandenburg, 2005)
;
_computing_publication_material
;
Olex2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1515
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57289
_diffrn_reflns_theta_full        25.038
_diffrn_reflns_theta_max         25.038
_diffrn_reflns_theta_min         1.228
_exptl_absorpt_coefficient_mu    1.679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             8320
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0728P)²+32.5817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                4971
_reflns_number_total             8101
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fn3233sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        18334(2)
_cod_database_code               2020778
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.752
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.24042(2) 0.15405(2) 0.44302(4) 0.0289(2) Uani d 1 . .
Zn Zn2 0.15697(2) 0.20404(2) 0.43840(4) 0.0307(2) Uani d 1 . .
Zn Zn3 0.16534(2) 0.12251(2) 0.32299(5) 0.0354(2) Uani d 1 . .
Ca Ca1 0.2500 0.2500 0.2500 0.0267(4) Uani d 1 . .
O O1 0.28138(12) 0.20906(12) 0.3398(3) 0.0358(11) Uani d 1 . .
O O2 0.29626(12) 0.15413(13) 0.4067(3) 0.0404(11) Uani d 1 . .
O O3 0.60114(14) 0.19367(17) 0.0908(3) 0.0644(16) Uani d 1 . .
O O4 0.61299(15) 0.15123(19) 0.1922(3) 0.0740(18) Uani d 1 . .
O O5 0.33454(14) 0.31593(15) 0.9516(3) 0.0479(12) Uani d 1 . .
O O6 0.26748(14) 0.31780(15) 0.9546(3) 0.0476(12) Uani d 1 . .
O O7 0.29141(12) 0.30432(13) 0.2742(2) 0.0357(10) Uani d 1 . .
O O8 0.31138(13) 0.36806(12) 0.2880(3) 0.0401(11) Uani d 1 . .
O O9 0.20384(13) 0.26553(12) 0.3473(3) 0.0386(11) Uani d 1 . .
O O10 0.16336(14) 0.26140(13) 0.4514(3) 0.0481(13) Uani d 1 . .
O O11 0.23654(14) 0.59815(13) 0.5189(3) 0.0522(14) Uani d 1 . .
O O12 0.2046(6) 0.5803(3) 0.6265(8) 0.033(5) Uani d 0.50(4) A 1
O O12A 0.1808(10) 0.5877(7) 0.5889(18) 0.092(12) Uani d 0.50(4) A 2
O O13 0.19484(12) 0.17008(11) 0.3770(2) 0.0261(9) Uani d 1 . .
H H13 0.2003(17) 0.1787(17) 0.3325(16) 0.031 Uiso d 1 . .
O O14 0.1374(2) 0.07056(17) 0.2861(4) 0.089(2) Uani d 1 . .
H H14A 0.1563(13) 0.0548(18) 0.278(5) 0.133 Uiso d 1 . .
H H14B 0.125(2) 0.0774(18) 0.245(3) 0.133 Uiso d 1 . .
O O15 0.1356(3) 0.1100(3) 0.4544(7) 0.067(3) Uani d 0.5 . .
H H15A 0.1483 0.1206 0.4941 0.100 Uiso d 0.5 . .
H H15B 0.1125 0.1224 0.4652 0.100 Uiso d 0.5 . .
C C1 0.30610(17) 0.18275(18) 0.3587(4) 0.0294(14) Uani d 1 . .
C C2 0.34812(17) 0.18305(18) 0.3266(4) 0.0302(14) Uani d 1 . .
C C3 0.36269(18) 0.21716(19) 0.2896(4) 0.0372(16) Uani d 1 . .
H H3 0.3466 0.2401 0.2864 0.034(17) Uiso calc 1 . .
C C4 0.40152(19) 0.2176(2) 0.2567(4) 0.0452(18) Uani d 1 . .
H H4 0.4114 0.2408 0.2326 0.054 Uiso calc 1 . .
C C5 0.42516(19) 0.1832(2) 0.2600(4) 0.0427(18) Uani d 1 . .
C C6 0.4098(2) 0.1495(2) 0.2959(5) 0.051(2) Uani d 1 . .
H H6 0.4254 0.1262 0.2972 0.061 Uiso calc 1 . .
C C7 0.37145(19) 0.14876(19) 0.3308(4) 0.0404(17) Uani d 1 . .
H H7 0.3620 0.1257 0.3562 0.048 Uiso calc 1 . .
C C8 0.4968(2) 0.1698(3) 0.2791(5) 0.085(3) Uani d 1 . .
H H8 0.4901 0.1639 0.3320 0.102 Uiso calc 1 . .
C C9 0.4672(2) 0.1819(2) 0.2282(5) 0.055(2) Uani d 1 . .
C C10 0.4775(2) 0.1922(2) 0.1498(5) 0.059(2) Uani d 1 . .
C C11 0.4463(3) 0.2024(3) 0.0848(7) 0.104(4) Uani d 1 . .
H H11A 0.4374 0.2297 0.0914 0.157 Uiso calc 1 . .
H H11B 0.4236 0.1845 0.0896 0.157 Uiso calc 1 . .
H H11C 0.4583 0.1992 0.0329 0.157 Uiso calc 1 . .
C C12 0.5366(2) 0.1660(3) 0.2547(6) 0.094(4) Uani d 1 . .
H H12 0.5560 0.1560 0.2898 0.112 Uiso calc 1 . .
C C13 0.5473(2) 0.1773(3) 0.1775(5) 0.061(2) Uani d 1 . .
C C14 0.5176(2) 0.1905(2) 0.1254(5) 0.062(2) Uani d 1 . .
H H14 0.5245 0.1982 0.0736 0.074 Uiso calc 1 . .
C C15 0.5905(2) 0.1733(3) 0.1513(5) 0.058(2) Uani d 1 . .
C C16 0.3004(2) 0.31616(19) 0.9178(4) 0.0384(16) Uani d 1 . .
C C17 0.3000(2) 0.3161(2) 0.8287(4) 0.0437(17) Uani d 1 . .
C C18 0.3349(2) 0.3212(3) 0.7849(4) 0.061(2) Uani d 1 . .
H H18 0.3595 0.3229 0.8114 0.073 Uiso calc 1 . .
C C19 0.3340(2) 0.3236(3) 0.7022(4) 0.068(3) Uani d 1 . .
H H19 0.3577 0.3280 0.6739 0.082 Uiso calc 1 . .
C C20 0.2980(2) 0.3196(2) 0.6614(4) 0.053(2) Uani d 1 . .
C C21 0.2628(2) 0.3133(3) 0.7054(5) 0.068(3) Uani d 1 . .
H H21 0.2383 0.3099 0.6790 0.082 Uiso calc 0.611(13) B 31
C C22 0.2641(2) 0.3123(3) 0.7881(4) 0.062(2) Uani d 1 . .
H H22 0.2402 0.3089 0.8169 0.074 Uiso calc 1 . .
C C23 0.2964(2) 0.3226(2) 0.5715(4) 0.052(2) Uani d 1 . .
C C24 0.2954(2) 0.3608(2) 0.5362(4) 0.053(2) Uani d 1 . .
H H24 0.2942 0.3837 0.5682 0.064 Uiso calc 1 . .
C C25 0.2962(2) 0.3644(2) 0.4547(4) 0.0472(18) Uani d 1 . .
H H25 0.2962 0.3900 0.4317 0.057 Uiso calc 1 . .
C C26 0.29703(18) 0.3311(2) 0.4062(4) 0.0342(15) Uani d 1 . .
C C27 0.2971(2) 0.2932(2) 0.4413(4) 0.0505(19) Uani d 1 . .
H H27 0.2974 0.2703 0.4092 0.061 Uiso calc 1 . .
C C28 0.2968(3) 0.2895(2) 0.5235(4) 0.057(2) Uani d 1 . .
H H28 0.2973 0.2631 0.5473 0.069 Uiso d 0.389(13) B 2
C C29 0.29998(18) 0.3347(2) 0.3170(4) 0.0343(15) Uani d 1 . .
C C30 0.3059(5) 0.2473(4) 0.5579(9) 0.086(5) Uani d 0.611(13) B 1
H H30A 0.2925 0.2442 0.6085 0.130 Uiso calc 0.611(13) B 1
H H30B 0.3345 0.2443 0.5653 0.130 Uiso calc 0.611(13) B 1
H H30C 0.2964 0.2270 0.5213 0.130 Uiso calc 0.611(13) B 1
C C30B 0.2199(6) 0.3095(10) 0.6691(17) 0.127(11) Uani d 0.389(13) B 2
H H30D 0.2216 0.3105 0.6117 0.190 Uiso calc 0.389(13) B 2
H H30E 0.2082 0.2843 0.6852 0.190 Uiso calc 0.389(13) B 2
H H30F 0.2033 0.3313 0.6879 0.190 Uiso calc 0.389(13) B 2
C C31 0.18550(19) 0.28138(18) 0.4030(4) 0.0335(15) Uani d 1 . .
C C32 0.18834(18) 0.32579(18) 0.4178(4) 0.0335(15) Uani d 1 . .
C C33 0.1810(2) 0.3423(2) 0.4930(5) 0.060(2) Uani d 1 . .
H H33 0.1731 0.3255 0.5348 0.072 Uiso calc 1 . .
C C34 0.1850(2) 0.3829(2) 0.5069(5) 0.064(2) Uani d 1 . .
H H34 0.1800 0.3932 0.5577 0.077 Uiso calc 1 . .
C C35 0.1966(2) 0.4086(2) 0.4447(5) 0.0470(18) Uani d 1 . .
C C36 0.20358(19) 0.39279(19) 0.3701(4) 0.0388(16) Uani d 1 . .
C C37 0.19987(19) 0.35183(19) 0.3577(4) 0.0390(16) Uani d 1 . .
H H37 0.2053 0.3414 0.3071 0.047 Uiso calc 1 . .
C C38 0.2008(2) 0.4523(2) 0.4669(4) 0.0459(18) Uani d 1 . .
C C39 0.1717(3) 0.4703(2) 0.5125(6) 0.073(3) Uani d 1 . .
H H39 0.1488 0.4558 0.5264 0.088 Uiso calc 1 . .
C C40 0.2093(2) 0.5322(2) 0.5186(5) 0.056(2) Uani d 1 . .
C C41 0.1758(3) 0.5102(2) 0.5389(6) 0.078(3) Uani d 1 . .
H H41 0.1558 0.5218 0.5702 0.094 Uiso calc 1 . .
C C42 0.2373(2) 0.5151(2) 0.4696(5) 0.059(2) Uani d 1 . .
H H42 0.2591 0.5305 0.4520 0.071 Uiso calc 1 . .
C C43 0.2341(2) 0.4754(2) 0.4456(5) 0.056(2) Uani d 1 . .
H H43 0.2545 0.4639 0.4148 0.067 Uiso calc 1 . .
C C44 0.2143(3) 0.5745(2) 0.5511(5) 0.061(2) Uani d 1 . .
C C45 0.2161(3) 0.4180(3) 0.2977(7) 0.103(4) Uani d 1 . .
H H45A 0.2047 0.4066 0.2499 0.154 Uiso calc 1 . .
H H45B 0.2450 0.4182 0.2934 0.154 Uiso calc 1 . .
H H45C 0.2065 0.4451 0.3042 0.154 Uiso calc 1 . .
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'
Ca Ca 0.2262 0.3064 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Zn1 O6 . 13_556 113.3(2) y
O2 Zn1 O11 . 14_546 99.44(19) ?
O11 Zn1 O6 14_546 13_556 99.1(2) y
O13 Zn1 O2 . . 124.24(17) ?
O13 Zn1 O6 . 13_556 105.02(18) ?
O13 Zn1 O11 . 14_546 112.99(18) y
O3 Zn2 O5 10_556 13_556 108.1(2) y
O3 Zn2 O13 10_556 . 112.01(19) y
O5 Zn2 O13 13_556 . 101.57(18) ?
O10 Zn2 O3 . 10_556 107.9(2) y
O10 Zn2 O5 . 13_556 102.2(2) ?
O10 Zn2 O13 . . 123.53(17) ?
O4 Zn3 O8 10_556 13 98.1(2) y
O4 Zn3 O12 10_556 14_546 155.9(6) ?
O4 Zn3 O13 10_556 . 95.91(19) ?
O4 Zn3 O14 10_556 . 88.3(2) ?
O4 Zn3 O15 10_556 . 81.0(3) ?
O8 Zn3 O12 13 14_546 103.5(6) y
O8 Zn3 O13 13 . 95.77(16) ?
O8 Zn3 O14 13 . 91.6(2) ?
O8 Zn3 O15 13 . 178.2(3) ?
O12 Zn3 O15 14_546 . 77.0(6) y
O12A Zn3 O4 14_546 10_556 127.6(13) ?
O12A Zn3 O8 14_546 13 133.1(14) ?
O12A Zn3 O13 14_546 . 89.9(5) ?
O12A Zn3 O14 14_546 . 81.2(5) ?
O12A Zn3 O15 14_546 . 47.5(14) ?
O13 Zn3 O12 . 14_546 92.3(3) ?
O13 Zn3 O15 . . 85.9(3) ?
O14 Zn3 O12 . 14_546 80.7(4) ?
O14 Zn3 O13 . . 170.9(2) ?
O14 Zn3 O15 . . 86.9(3) ?
O1 Ca1 O1 13 . 180.00(16) y
O1 Ca1 O7 13 13 94.50(15) ?
O1 Ca1 O7 . . 94.50(15) y
O1 Ca1 O7 . 13 85.50(15) ?
O1 Ca1 O7 13 . 85.50(15) ?
O1 Ca1 O9 . 13 91.55(15) ?
O1 Ca1 O9 . . 88.44(15) ?
O1 Ca1 O9 13 . 91.56(15) ?
O1 Ca1 O9 13 13 88.44(15) ?
O7 Ca1 O7 13 . 180.0(2) ?
O9 Ca1 O7 . . 95.64(15) y
O9 Ca1 O7 13 . 84.36(15) ?
O9 Ca1 O7 . 13 84.36(15) ?
O9 Ca1 O7 13 13 95.64(15) ?
O9 Ca1 O9 13 . 180.0 ?
C1 O1 Ca1 . . 153.1(4) ?
C1 O2 Zn1 . . 115.9(4) ?
C15 O3 Zn2 . 10_656 124.1(5) ?
C15 O4 Zn3 . 10_656 136.9(5) ?
C16 O5 Zn2 . 13_556 123.1(4) ?
C16 O6 Zn1 . 13_556 124.2(4) ?
C29 O7 Ca1 . . 148.8(4) ?
C29 O8 Zn3 . 13 126.7(4) ?
C31 O9 Ca1 . . 164.4(4) ?
C31 O10 Zn2 . . 120.2(4) ?
C44 O11 Zn1 . 14_556 120.8(5) ?
C44 O12 Zn3 . 14_556 129.6(11) ?
C44 O12A Zn3 . 14_556 140(2) ?
Zn1 O13 Zn2 . . 110.90(19) ?
Zn1 O13 Zn3 . . 114.02(18) ?
Zn1 O13 H13 . . 116(4) ?
Zn2 O13 Zn3 . . 111.18(18) ?
Zn2 O13 H13 . . 114(4) ?
Zn3 O13 H13 . . 88(4) ?
Zn3 O14 H14A . . 104(5) ?
Zn3 O14 H14B . . 104(5) ?
H14A O14 H14B . . 114(2) ?
Zn3 O15 H15A . . 115.3 ?
Zn3 O15 H15B . . 117.0 ?
H15A O15 H15B . . 94.5 ?
O1 C1 O2 . . 120.8(5) ?
O1 C1 C2 . . 121.4(6) ?
O2 C1 C2 . . 117.8(5) ?
C3 C2 C1 . . 119.6(5) ?
C3 C2 C7 . . 120.3(6) ?
C7 C2 C1 . . 120.0(6) ?
C2 C3 H3 . . 119.8 ?
C2 C3 C4 . . 120.4(6) ?
C4 C3 H3 . . 119.8 ?
C3 C4 H4 . . 120.1 ?
C5 C4 C3 . . 119.8(6) ?
C5 C4 H4 . . 120.1 ?
C4 C5 C9 . . 122.6(6) ?
C6 C5 C4 . . 118.6(6) ?
C6 C5 C9 . . 118.7(6) ?
C5 C6 H6 . . 118.8 ?
C5 C6 C7 . . 122.5(6) ?
C7 C6 H6 . . 118.8 ?
C2 C7 C6 . . 118.3(6) ?
C2 C7 H7 . . 120.8 ?
C6 C7 H7 . . 120.8 ?
C9 C8 H8 . . 119.0 ?
C9 C8 C12 . . 122.1(8) ?
C12 C8 H8 . . 119.0 ?
C8 C9 C5 . . 117.4(7) ?
C8 C9 C10 . . 118.8(7) ?
C10 C9 C5 . . 123.8(7) ?
C9 C10 C11 . . 123.4(7) ?
C14 C10 C9 . . 119.9(7) ?
C14 C10 C11 . . 116.5(8) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C8 C12 H12 . . 120.3 ?
C13 C12 C8 . . 119.4(8) ?
C13 C12 H12 . . 120.3 ?
C12 C13 C15 . . 119.3(7) ?
C14 C13 C12 . . 119.1(7) ?
C14 C13 C15 . . 121.5(7) ?
C10 C14 H14 . . 119.7 ?
C13 C14 C10 . . 120.6(7) ?
C13 C14 H14 . . 119.7 ?
O3 C15 C13 . . 116.9(7) ?
O4 C15 O3 . . 125.6(7) ?
O4 C15 C13 . . 117.5(7) ?
O5 C16 C17 . . 117.1(6) ?
O6 C16 O5 . . 124.1(6) ?
O6 C16 C17 . . 118.8(6) ?
C18 C17 C16 . . 121.4(7) ?
C22 C17 C16 . . 120.1(7) ?
C22 C17 C18 . . 118.5(7) ?
C17 C18 H18 . . 119.5 ?
C17 C18 C19 . . 121.1(7) ?
C19 C18 H18 . . 119.5 ?
C18 C19 H19 . . 119.8 ?
C20 C19 C18 . . 120.4(8) ?
C20 C19 H19 . . 119.8 ?
C19 C20 C21 . . 118.5(7) ?
C19 C20 C23 . . 121.1(7) ?
C21 C20 C23 . . 120.4(7) ?
C20 C21 H21 . . 119.8 ?
C20 C21 C30B . . 125.0(13) ?
C22 C21 C20 . . 120.4(7) ?
C22 C21 H21 . . 119.8 ?
C22 C21 C30B . . 114.6(13) ?
C17 C22 C21 . . 121.0(7) ?
C17 C22 H22 . . 119.5 ?
C21 C22 H22 . . 119.5 ?
C24 C23 C20 . . 118.9(7) ?
C28 C23 C20 . . 122.1(7) ?
C28 C23 C24 . . 118.9(7) ?
C23 C24 H24 . . 120.0 ?
C25 C24 C23 . . 120.0(7) ?
C25 C24 H24 . . 120.0 ?
C24 C25 H25 . . 119.5 ?
C24 C25 C26 . . 121.1(7) ?
C26 C25 H25 . . 119.5 ?
C25 C26 C27 . . 118.8(6) ?
C25 C26 C29 . . 121.6(6) ?
C27 C26 C29 . . 119.5(6) ?
C26 C27 H27 . . 119.9 ?
C28 C27 C26 . . 120.2(7) ?
C28 C27 H27 . . 119.9 ?
C23 C28 C27 . . 120.9(7) ?
C23 C28 H28 . . 119.5 ?
C23 C28 C30 . . 121.1(8) ?
C27 C28 H28 . . 119.6 ?
C27 C28 C30 . . 116.8(8) ?
O7 C29 C26 . . 118.8(6) ?
O8 C29 O7 . . 123.2(6) ?
O8 C29 C26 . . 118.1(6) ?
C28 C30 H30A . . 109.5 ?
C28 C30 H30B . . 109.5 ?
C28 C30 H30C . . 109.5 ?
H30A C30 H30B . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
C21 C30B H30D . . 109.5 ?
C21 C30B H30E . . 109.5 ?
C21 C30B H30F . . 109.5 ?
H30D C30B H30E . . 109.5 ?
H30D C30B H30F . . 109.5 ?
H30E C30B H30F . . 109.5 ?
O9 C31 O10 . . 122.8(6) ?
O9 C31 C32 . . 121.0(6) ?
O10 C31 C32 . . 116.2(6) ?
C33 C32 C31 . . 121.7(6) ?
C37 C32 C31 . . 121.0(6) ?
C37 C32 C33 . . 117.3(6) ?
C32 C33 H33 . . 119.3 ?
C34 C33 C32 . . 121.4(7) ?
C34 C33 H33 . . 119.3 ?
C33 C34 H34 . . 120.0 ?
C33 C34 C35 . . 120.0(7) ?
C35 C34 H34 . . 120.0 ?
C34 C35 C38 . . 115.6(7) ?
C36 C35 C34 . . 119.2(6) ?
C36 C35 C38 . . 125.2(7) ?
C35 C36 C37 . . 119.8(6) ?
C35 C36 C45 . . 123.8(7) ?
C37 C36 C45 . . 116.4(7) ?
C32 C37 C36 . . 122.2(6) ?
C32 C37 H37 . . 118.9 ?
C36 C37 H37 . . 118.9 ?
C39 C38 C35 . . 119.6(7) ?
C39 C38 C43 . . 117.5(6) ?
C43 C38 C35 . . 122.9(6) ?
C38 C39 H39 . . 119.3 ?
C38 C39 C41 . . 121.3(7) ?
C41 C39 H39 . . 119.3 ?
C41 C40 C44 . . 119.6(7) ?
C42 C40 C41 . . 118.7(7) ?
C42 C40 C44 . . 121.6(7) ?
C39 C41 H41 . . 119.9 ?
C40 C41 C39 . . 120.3(7) ?
C40 C41 H41 . . 119.9 ?
C40 C42 H42 . . 119.4 ?
C40 C42 C43 . . 121.2(7) ?
C43 C42 H42 . . 119.4 ?
C38 C43 H43 . . 119.6 ?
C42 C43 C38 . . 120.9(7) ?
C42 C43 H43 . . 119.6 ?
O11 C44 O12 . . 118.8(9) ?
O11 C44 O12A . . 119.9(11) ?
O11 C44 C40 . . 120.9(7) ?
O12 C44 C40 . . 116.9(8) ?
O12A C44 C40 . . 112.2(8) ?
C36 C45 H45A . . 109.5 ?
C36 C45 H45B . . 109.5 ?
C36 C45 H45C . . 109.5 ?
H45A C45 H45B . . 109.5 ?
H45A C45 H45C . . 109.5 ?
H45B C45 H45C . . 109.5 ?
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
Zn1 O2 . 1.948(4) y
Zn1 O6 13_556 1.964(4) y
Zn1 O11 14_546 1.963(4) y
Zn1 O13 . 1.944(4) ?
Zn2 O3 10_556 1.945(5) y
Zn2 O5 13_556 1.971(5) y
Zn2 O10 . 1.926(4) y
Zn2 O13 . 1.973(4) ?
Zn3 O4 10_556 1.996(5) y
Zn3 O8 13 2.030(4) y
Zn3 O12 14_546 2.090(11) ?
Zn3 O12A 14_546 1.937(13) ?
Zn3 O13 . 2.063(4) ?
Zn3 O14 . 2.049(6) ?
Zn3 O15 . 2.439(11) ?
Ca1 O1 13 2.274(4) ?
Ca1 O1 . 2.274(4) y
Ca1 O7 13 2.300(4) ?
Ca1 O7 . 2.300(4) y
Ca1 O9 . 2.289(4) ?
Ca1 O9 13 2.289(4) ?
O1 C1 . 1.238(7) ?
O2 C1 . 1.284(7) ?
O3 Zn2 10_656 1.944(5) ?
O3 C15 . 1.263(9) ?
O4 Zn3 10_656 1.995(5) ?
O4 C15 . 1.249(9) ?
O5 Zn2 13_556 1.971(5) ?
O5 C16 . 1.265(8) ?
O6 Zn1 13_556 1.964(4) ?
O6 C16 . 1.254(8) ?
O7 C29 . 1.268(7) ?
O8 Zn3 13 2.030(4) ?
O8 C29 . 1.263(7) ?
O9 C31 . 1.228(7) ?
O10 C31 . 1.277(7) ?
O11 Zn1 14_556 1.963(4) ?
O11 C44 . 1.203(8) ?
O12 Zn3 14_556 2.090(11) ?
O12 C44 . 1.312(14) ?
O12A Zn3 14_556 1.937(13) ?
O12A C44 . 1.35(2) ?
O13 H13 . 0.815(10) ?
O14 H14A . 0.825(10) ?
O14 H14B . 0.825(10) ?
O15 H15A . 0.8579 ?
O15 H15B . 0.8875 ?
C1 C2 . 1.492(8) ?
C2 C3 . 1.376(8) ?
C2 C7 . 1.377(8) ?
C3 H3 . 0.9300 ?
C3 C4 . 1.400(9) ?
C4 H4 . 0.9300 ?
C4 C5 . 1.383(9) ?
C5 C6 . 1.366(9) ?
C5 C9 . 1.492(9) ?
C6 H6 . 0.9300 ?
C6 C7 . 1.397(9) ?
C7 H7 . 0.9300 ?
C8 H8 . 0.9300 ?
C8 C9 . 1.357(10) ?
C8 C12 . 1.388(10) ?
C9 C10 . 1.394(10) ?
C10 C11 . 1.536(12) ?
C10 C14 . 1.391(9) ?
C11 H11A . 0.9600 ?
C11 H11B . 0.9600 ?
C11 H11C . 0.9600 ?
C12 H12 . 0.9300 ?
C12 C13 . 1.387(11) ?
C13 C14 . 1.384(10) ?
C13 C15 . 1.503(9) ?
C14 H14 . 0.9300 ?
C16 C17 . 1.486(9) ?
C17 C18 . 1.380(10) ?
C17 C22 . 1.375(10) ?
C18 H18 . 0.9300 ?
C18 C19 . 1.382(10) ?
C19 H19 . 0.9300 ?
C19 C20 . 1.380(10) ?
C20 C21 . 1.393(10) ?
C20 C23 . 1.503(10) ?
C21 H21 . 0.9300 ?
C21 C22 . 1.381(10) ?
C21 C30B . 1.552(15) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.395(10) ?
C23 C28 . 1.360(10) ?
C24 H24 . 0.9300 ?
C24 C25 . 1.366(9) ?
C25 H25 . 0.9300 ?
C25 C26 . 1.369(9) ?
C26 C27 . 1.385(9) ?
C26 C29 . 1.498(8) ?
C27 H27 . 0.9300 ?
C27 C28 . 1.378(10) ?
C28 H28 . 0.9599 ?
C28 C30 . 1.542(13) ?
C30 H30A . 0.9600 ?
C30 H30B . 0.9600 ?
C30 H30C . 0.9600 ?
C30B H30D . 0.9600 ?
C30B H30E . 0.9600 ?
C30B H30F . 0.9600 ?
C31 C32 . 1.496(8) ?
C32 C33 . 1.391(9) ?
C32 C37 . 1.377(9) ?
C33 H33 . 0.9300 ?
C33 C34 . 1.370(9) ?
C34 H34 . 0.9300 ?
C34 C35 . 1.396(10) ?
C35 C36 . 1.370(9) ?
C35 C38 . 1.501(9) ?
C36 C37 . 1.379(8) ?
C36 C45 . 1.527(12) ?
C37 H37 . 0.9300 ?
C38 C39 . 1.366(10) ?
C38 C43 . 1.390(9) ?
C39 H39 . 0.9300 ?
C39 C41 . 1.402(10) ?
C40 C41 . 1.368(10) ?
C40 C42 . 1.361(10) ?
C40 C44 . 1.512(9) ?
C41 H41 . 0.9300 ?
C42 H42 . 0.9300 ?
C42 C43 . 1.381(9) ?
C43 H43 . 0.9300 ?
C45 H45A . 0.9600 ?
C45 H45B . 0.9600 ?
C45 H45C . 0.9600 ?
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
O13 H13 O7 13 0.815(10) 1.888(13) 2.701(6) 175(6)
O13 H13 O8 13 0.815(10) 2.57(5) 3.036(6) 118(5)
O14 H14A O11 16_656 0.825(10) 2.40(5) 2.971(7) 127(6)
O14 H14B O2 7_444 0.825(10) 2.05(5) 2.685(7) 134(6)
O15 H15A O5 13_556 0.86 2.36 3.075(12) 140.9
O15 H15B O3 10_556 0.89 2.57 3.092(12) 118.4
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
Zn1 O2 C1 O1 . 2.4(8)
Zn1 O2 C1 C2 . -177.5(4)
Zn1 O6 C16 O5 13_556 31.8(9)
Zn1 O6 C16 C17 13_556 -145.6(5)
Zn1 O11 C44 O12 14_556 -25.5(14)
Zn1 O11 C44 O12A 14_556 28(2)
Zn1 O11 C44 C40 14_556 176.0(6)
Zn2 O3 C15 O4 10_656 -13.6(13)
Zn2 O3 C15 C13 10_656 164.2(6)
Zn2 O5 C16 O6 13_556 26.2(9)
Zn2 O5 C16 C17 13_556 -156.4(5)
Zn2 O10 C31 O9 . -0.8(9)
Zn2 O10 C31 C32 . 179.6(4)
Zn3 O4 C15 O3 10_656 -22.0(15)
Zn3 O4 C15 C13 10_656 160.2(6)
Zn3 O8 C29 O7 13 -19.6(9)
Zn3 O8 C29 C26 13 159.6(4)
Zn3 O12 C44 O11 14_556 74.2(19)
Zn3 O12 C44 C40 14_556 -126.4(11)
Zn3 O12A C44 O11 14_556 -61(4)
Zn3 O12A C44 C40 14_556 148(3)
Ca1 O1 C1 O2 . -136.0(7)
Ca1 O1 C1 C2 . 43.8(12)
Ca1 O7 C29 O8 . -139.1(6)
Ca1 O7 C29 C26 . 41.7(11)
Ca1 O9 C31 O10 . -149.6(13)
Ca1 O9 C31 C32 . 30(2)
O1 C1 C2 C3 . 14.2(9)
O1 C1 C2 C7 . -162.8(6)
O2 C1 C2 C3 . -166.0(6)
O2 C1 C2 C7 . 17.0(9)
O5 C16 C17 C18 . -8.6(10)
O5 C16 C17 C22 . 173.5(7)
O6 C16 C17 C18 . 169.0(7)
O6 C16 C17 C22 . -8.9(11)
O9 C31 C32 C33 . -156.2(7)
O9 C31 C32 C37 . 21.4(10)
O10 C31 C32 C33 . 23.4(10)
O10 C31 C32 C37 . -159.0(6)
C1 C2 C3 C4 . -177.8(6)
C1 C2 C7 C6 . 176.3(6)
C2 C3 C4 C5 . 1.2(11)
C3 C2 C7 C6 . -0.7(10)
C3 C4 C5 C6 . -0.1(11)
C3 C4 C5 C9 . -178.3(7)
C4 C5 C6 C7 . -1.4(12)
C4 C5 C9 C8 . 125.0(9)
C4 C5 C9 C10 . -55.0(12)
C5 C6 C7 C2 . 1.8(12)
C5 C9 C10 C11 . -6.0(14)
C5 C9 C10 C14 . 179.3(8)
C6 C5 C9 C8 . -53.2(12)
C6 C5 C9 C10 . 126.8(9)
C7 C2 C3 C4 . -0.8(10)
C8 C9 C10 C11 . 174.0(9)
C8 C9 C10 C14 . -0.7(14)
C8 C12 C13 C14 . -2.8(16)
C8 C12 C13 C15 . 179.7(9)
C9 C5 C6 C7 . 176.8(7)
C9 C8 C12 C13 . 4.3(18)
C9 C10 C14 C13 . 2.1(14)
C11 C10 C14 C13 . -172.9(8)
C12 C8 C9 C5 . 177.4(9)
C12 C8 C9 C10 . -2.6(16)
C12 C13 C14 C10 . -0.3(14)
C12 C13 C15 O3 . -160.9(9)
C12 C13 C15 O4 . 17.1(14)
C14 C13 C15 O3 . 21.7(13)
C14 C13 C15 O4 . -160.4(9)
C15 C13 C14 C10 . 177.1(8)
C16 C17 C18 C19 . -175.9(8)
C16 C17 C22 C21 . 178.1(8)
C17 C18 C19 C20 . -2.4(14)
C18 C17 C22 C21 . 0.1(13)
C18 C19 C20 C21 . 0.6(14)
C18 C19 C20 C23 . 179.3(8)
C19 C20 C21 C22 . 1.5(14)
C19 C20 C21 C30B . 178.1(17)
C19 C20 C23 C24 . -81.6(10)
C19 C20 C23 C28 . 96.7(10)
C20 C21 C22 C17 . -1.9(14)
C20 C23 C24 C25 . 176.4(7)
C20 C23 C28 C27 . -177.1(7)
C20 C23 C28 C30 . -9.9(14)
C21 C20 C23 C24 . 97.1(10)
C21 C20 C23 C28 . -84.6(11)
C22 C17 C18 C19 . 2.0(13)
C23 C20 C21 C22 . -177.2(8)
C23 C20 C21 C30B . -1(2)
C23 C24 C25 C26 . 1.5(12)
C24 C23 C28 C27 . 1.2(12)
C24 C23 C28 C30 . 168.4(10)
C24 C25 C26 C27 . -0.1(11)
C24 C25 C26 C29 . -176.9(7)
C25 C26 C27 C28 . -0.7(11)
C25 C26 C29 O7 . -163.9(6)
C25 C26 C29 O8 . 16.8(9)
C26 C27 C28 C23 . 0.1(12)
C26 C27 C28 C30 . -167.6(9)
C27 C26 C29 O7 . 19.3(9)
C27 C26 C29 O8 . -160.0(6)
C28 C23 C24 C25 . -2.0(12)
C29 C26 C27 C28 . 176.2(7)
C30B C21 C22 C17 . -178.8(15)
C31 C32 C33 C34 . 177.7(7)
C31 C32 C37 C36 . -178.6(6)
C32 C33 C34 C35 . 0.3(13)
C33 C32 C37 C36 . -0.9(10)
C33 C34 C35 C36 . 0.3(12)
C33 C34 C35 C38 . -179.0(7)
C34 C35 C36 C37 . -1.2(11)
C34 C35 C36 C45 . 179.6(8)
C34 C35 C38 C39 . -45.1(11)
C34 C35 C38 C43 . 132.3(8)
C35 C36 C37 C32 . 1.5(10)
C35 C38 C39 C41 . 175.8(9)
C35 C38 C43 C42 . -177.8(8)
C36 C35 C38 C39 . 135.7(9)
C36 C35 C38 C43 . -46.9(12)
C37 C32 C33 C34 . 0.0(12)
C38 C35 C36 C37 . 178.0(7)
C38 C35 C36 C45 . -1.2(12)
C38 C39 C41 C40 . 0.5(16)
C39 C38 C43 C42 . -0.3(13)
C40 C42 C43 C38 . 3.8(14)
C41 C40 C42 C43 . -5.1(14)
C41 C40 C44 O11 . -159.7(9)
C41 C40 C44 O12 . 41.4(16)
C41 C40 C44 O12A . -9(2)
C42 C40 C41 C39 . 2.9(15)
C42 C40 C44 O11 . 20.7(14)
C42 C40 C44 O12 . -138.2(13)
C42 C40 C44 O12A . 171(2)
C43 C38 C39 C41 . -1.8(14)
C44 C40 C41 C39 . -176.7(9)
C44 C40 C42 C43 . 174.6(8)
C45 C36 C37 C32 . -179.2(7)

_cod_database_fobs_code 2020778
