#------------------------------------------------------------------------------
#$Date: 2021-07-07 07:44:27 +0300 (Wed, 07 Jul 2021) $
#$Revision: 267320 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/88/2108834.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_2108834
loop_
_publ_author_name
'Marabello, Domenica'
'Antoniotti, Paola'
'Benzi, Paola'
'Beccari, Fabio'
'Canepa, Carlo'
'Cariati, Elena'
'Cioci, Alma'
'Lo Presti, Leonardo'
_publ_section_title
;
 Crystal structure or chemical composition of salt--sugar-based
 metal--organic frameworks: what are the nonlinear optical properties due
 to?
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520621004637
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         '2(I), C12 H28 Ca O12'
_chemical_formula_sum            'C12 H28 Ca I2 O12'
_chemical_formula_weight         658.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.233(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6384(3)
_cell_length_b                   14.4621(4)
_cell_length_c                   10.7490(3)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.8760
_cell_measurement_theta_min      4.3350
_cell_volume                     1121.14(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -73.00 -44.00   1.00    4.00    --  -42.64  77.00-150.00   29
  2  ω    -28.00  47.00   1.00    4.00    --   42.64 -57.00-150.00   75
  3  ω     11.00 115.00   1.00    4.00    --   42.64  77.00 -30.00  104
  4  ω    -19.00  30.00   1.00    4.00    --   42.64 -57.00  60.00   49
  5  ω     86.00 116.00   1.00   10.00    --   92.50  45.00-120.00   30
  6  ω     39.00 106.00   1.00   10.00    --   92.50 -70.00  -1.27   67
  7  ω     19.00 104.00   1.00   10.00    --   92.50 -70.00  77.61   85
  8  ω     72.00  98.00   1.00   10.00    --   92.50  45.00  90.00   26
  9  ω     70.00 122.00   1.00   10.00    --   92.50 -70.00 -92.78   52
 10  ω    110.00 136.00   1.00   10.00    --   92.50  45.00  90.00   26
 11  ω     21.00  61.00   1.00   10.00    --   92.50 -61.00 150.00   40
 12  ω     20.00 114.00   1.00   10.00    --   92.50 -70.00-157.10   94
 13  ω     16.00  60.00   1.00   10.00    --   92.50 -30.00   0.00   44
 14  ω    105.00 131.00   1.00   10.00    --   92.50  61.00-180.00   26
 15  ω     73.00  98.00   1.00   10.00    --   92.50  30.00  60.00   25
 16  ω     61.00  98.00   1.00   10.00    --   92.50 -70.00 120.55   37
 17  ω    106.00 163.00   1.00   10.00    --   92.50  45.00 -90.00   57
 18  ω    131.00 166.00   1.00   10.00    --   92.50  30.00  60.00   35
 19  ω     93.00 120.00   1.00   10.00    --   92.50  77.00 -30.00   27
 20  ω    126.00 162.00   1.00   10.00    --   92.50  45.00 -60.00   36
 21  ω     97.00 122.00   1.00   10.00    --   92.50  61.00  30.00   25
 22  ω    126.00 158.00   1.00   10.00    --   92.50  61.00  30.00   32
 23  ω     46.00  72.00   1.00   10.00    --   92.50 -61.00-120.00   26
 24  ω     74.00 109.00   1.00   10.00    --   92.50 -61.00 150.00   35
 25  ω     27.00  52.00   1.00   10.00    --   92.50 -45.00  30.00   25
 26  ω     90.00 116.00   1.00   10.00    --   92.50 -45.00  30.00   26
 27  ω     77.00 102.00   1.00   10.00    --   92.50  45.00 -90.00   25
 28  ω     96.00 121.00   1.00   10.00    --   92.50 -30.00   0.00   25
 29  ω     68.00 147.00   1.00   10.00    --   92.50  30.00  30.00   79
 30  ω     87.00 155.00   1.00   10.00    --   92.50  45.00 -30.00   68
 31  ω     37.00  63.00   1.00   10.00    --   92.50 -70.00 -92.78   26
 32  ω     96.00 122.00   1.00   10.00    --   92.50 -61.00-120.00   26
 33  ω     73.00  98.00   1.00   10.00    --   92.50 -66.00  25.21   25
 34  ω     58.00  83.00   1.00   10.00    --   92.50 -70.00-125.03   25
 35  ω     21.00  46.00   1.00   10.00    --   92.50 -67.00 -68.04   25
 36  ω     72.00  98.00   1.00   10.00    --   92.50 -70.00 -58.23   26
 37  ω     23.00  51.00   1.00   10.00    --   92.50 -70.00 -58.23   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0168014000
_diffrn_orient_matrix_UB_12      -0.0861180000
_diffrn_orient_matrix_UB_13      -0.0797024000
_diffrn_orient_matrix_UB_21      0.0906509000
_diffrn_orient_matrix_UB_22      -0.0535551000
_diffrn_orient_matrix_UB_23      0.1291305000
_diffrn_orient_matrix_UB_31      -0.1926682000
_diffrn_orient_matrix_UB_32      -0.0327776000
_diffrn_orient_matrix_UB_33      -0.0016926000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11076
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        66.914
_diffrn_reflns_theta_max         66.914
_diffrn_reflns_theta_min         4.356
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.519
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0316
_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)+(0.0436P)²+0.4062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.877
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                3590
_reflns_number_total             3737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            um5049sup1.cif
_cod_data_source_block           CaDgalI_new
_cod_original_cell_volume        1121.14(6)
_cod_database_code               2108834
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ca(C6H10O5)I2(H2O)2
_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.
;
_reflns_odcompleteness_completeness 98.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Ternary CH refined with riding coordinates:
 C1A(H1A), C1B(H1B), C3A(H3AA), C3B(H3BA), C4A(H4AA), C4B(H4BA), C5A(H5AA),
 C5B(H5BA)
2.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB)
2.d Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2B(H2B), O3A(H3A), O3B(H3B), O4A(H4A), O4B(H4B), O5A(H5A), O5B(H5B)
;
_olex2_submission_original_sample_id CaDGalI
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.660
_oxdiff_exptl_absorpt_empirical_full_min 0.727
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.77763(8) 0.68054(4) 0.72648(5) 0.04633(18) Uani 1 1 d . . . . .
I2 I 0.58728(8) 0.50584(4) 0.23699(5) 0.04716(18) Uani 1 1 d . . . . .
Ca1 Ca 0.4867(2) 0.38036(10) 0.73658(14) 0.0311(3) Uani 1 1 d . . . . .
O1A O 0.2193(8) 0.6599(3) 0.4514(5) 0.0358(12) Uani 1 1 d . . . . .
O1B O 1.0320(11) 0.4528(5) 0.9154(9) 0.0591(19) Uani 1 1 d . . . . .
O1W O 0.6723(12) 0.4393(6) 0.6068(8) 0.066(2) Uani 1 1 d . . . . .
H1WA H 0.697158 0.496717 0.613025 0.13(8) Uiso 1 1 d R . . . .
H1WB H 0.694508 0.424477 0.536915 0.15(9) Uiso 1 1 d R . . . .
O2A O 0.1838(10) 0.6122(4) 0.2418(6) 0.0455(15) Uani 1 1 d . . . . .
H2A H 0.281822 0.585125 0.252069 0.05(3) Uiso 1 1 calc R . . . .
O2B O 0.7224(8) 0.4818(4) 0.8893(6) 0.0401(14) Uani 1 1 d . . . . .
H2B H 0.726877 0.528782 0.847808 0.060 Uiso 1 1 calc R U . . .
O2W O 0.4827(11) 0.2625(6) 0.5801(7) 0.061(2) Uani 1 1 d . . . . .
H2WA H 0.592408 0.242960 0.593747 0.092 Uiso 1 1 d R U . . .
H2WB H 0.417308 0.293010 0.513317 0.092 Uiso 1 1 d R U . . .
O3A O 0.1660(8) 0.3996(4) 0.5857(5) 0.0365(13) Uani 1 1 d . . . . .
H3A H 0.096832 0.358615 0.544315 0.055 Uiso 1 1 calc R U . . .
O3B O 0.7534(8) 0.2843(4) 0.8472(6) 0.0386(13) Uani 1 1 d . . . . .
H3B H 0.754027 0.230980 0.821540 0.058 Uiso 1 1 calc R U . . .
O4A O 0.3817(8) 0.5419(4) 0.6864(6) 0.0392(13) Uani 1 1 d . . . . .
H4A H 0.442011 0.578222 0.658197 0.059 Uiso 1 1 calc R U . . .
O4B O 1.3771(8) 0.3993(4) 0.9217(6) 0.0400(13) Uani 1 1 d . . . . .
H4B H 1.418771 0.436388 0.981894 0.09(5) Uiso 1 1 calc R . . . .
O5A O 0.1637(11) 0.8193(4) 0.5844(7) 0.058(2) Uani 1 1 d . . . . .
H5A H 0.211256 0.863097 0.632060 0.087 Uiso 1 1 calc R U . . .
O5B O 1.3210(10) 0.2450(4) 0.7903(6) 0.0451(15) Uani 1 1 d . . . . .
H5B H 1.357937 0.195792 0.770187 0.05(3) Uiso 1 1 calc R . . . .
C1A C 0.1259(12) 0.5958(6) 0.3493(8) 0.0355(18) Uani 1 1 d . . . . .
H1A H -0.007597 0.607937 0.322820 0.043 Uiso 1 1 calc R U . . .
C1B C 0.9022(13) 0.4623(7) 0.9802(9) 0.045(2) Uani 1 1 d . . . . .
H1B H 0.940528 0.511109 1.046979 0.054 Uiso 1 1 calc R U . . .
C2A C 0.1614(13) 0.4979(6) 0.4029(8) 0.0392(19) Uani 1 1 d . . . . .
H2AA H 0.091758 0.454717 0.335684 0.047 Uiso 1 1 calc R U . . .
H2AB H 0.292045 0.483476 0.424612 0.047 Uiso 1 1 calc R U . . .
C2B C 0.8957(14) 0.3708(7) 1.0442(8) 0.045(2) Uani 1 1 d . . . . .
H2BA H 0.776650 0.360892 1.056105 0.054 Uiso 1 1 calc R U . . .
H2BB H 0.993300 0.365769 1.128783 0.054 Uiso 1 1 calc R U . . .
C3A C 0.1051(12) 0.4867(5) 0.5241(8) 0.0354(18) Uani 1 1 d . . . . .
H3AA H -0.030342 0.489968 0.498335 0.042 Uiso 1 1 calc R U . . .
C3B C 0.9256(11) 0.3041(6) 0.9455(8) 0.0345(17) Uani 1 1 d . . . . .
H3BA H 0.983189 0.247014 0.989407 0.041 Uiso 1 1 calc R U . . .
C4A C 0.1888(11) 0.5607(5) 0.6264(8) 0.0330(16) Uani 1 1 d . . . . .
H4AA H 0.129042 0.557778 0.694253 0.040 Uiso 1 1 calc R U . . .
C4B C 1.0590(12) 0.3560(6) 0.8900(8) 0.0366(18) Uani 1 1 d . . . . .
H4BA H 1.025144 0.345162 0.795023 0.044 Uiso 1 1 calc R U . . .
C5A C 0.1494(12) 0.6552(5) 0.5597(8) 0.0315(17) Uani 1 1 d . . . . .
H5AA H 0.014659 0.663560 0.524854 0.038 Uiso 1 1 calc R U . . .
C5B C 1.2621(12) 0.3332(6) 0.9581(8) 0.0385(19) Uani 1 1 d . . . . .
H5BA H 1.289182 0.335456 1.053719 0.046 Uiso 1 1 calc R U . . .
C6A C 0.2306(13) 0.7348(6) 0.6518(9) 0.042(2) Uani 1 1 d . . . . .
H6AA H 0.194131 0.730199 0.729869 0.050 Uiso 1 1 calc R U . . .
H6AB H 0.364875 0.733032 0.678869 0.050 Uiso 1 1 calc R U . . .
C6B C 1.3158(14) 0.2391(7) 0.9206(10) 0.045(2) Uani 1 1 d . . . . .
H6BA H 1.436383 0.221190 0.980649 0.055 Uiso 1 1 calc R U . . .
H6BB H 1.225736 0.193112 0.925312 0.055 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 7 5 0.0499
4 5 0 0.1135
-1 4 6 0.0691
-3 -6 -1 0.0584
0 9 0 0.0589
-3 8 1 0.0737
0 -6 5 0.0564
-1 6 -5 0.0311
1 -8 2 0.0262
-4 3 -2 0.0804
3 -3 3 0.0791
4 -3 -5 0.0886
-2 -7 -3 0.0489
0 -7 -5 0.0366
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
O1W Ca1 O2B 75.0(3) . . ?
O1W Ca1 H2WA 66.8 . . ?
O1W Ca1 H2WB 67.9 . . ?
O1W Ca1 O3A 102.8(3) . . ?
O1W Ca1 O4A 75.7(3) . . ?
O1W Ca1 O5B 146.8(3) . 1_455 ?
O2B Ca1 H2WA 120.5 . . ?
O2B Ca1 H2WB 141.2 . . ?
O2B Ca1 O5B 128.5(2) . 1_455 ?
O2W Ca1 O1W 73.8(3) . . ?
O2W Ca1 O2B 136.6(3) . . ?
O2W Ca1 H2WA 16.7 . . ?
O2W Ca1 H2WB 18.9 . . ?
O2W Ca1 O3A 80.7(2) . . ?
O2W Ca1 O3B 75.6(2) . . ?
O2W Ca1 O4A 126.4(3) . . ?
O2W Ca1 O4B 137.2(3) . 1_455 ?
O2W Ca1 O5B 73.4(3) . 1_455 ?
H2WA Ca1 H2WB 32.4 . . ?
O3A Ca1 O2B 135.7(2) . . ?
O3A Ca1 H2WA 97.1 . . ?
O3A Ca1 H2WB 66.0 . . ?
O3A Ca1 O4A 64.51(19) . . ?
O3A Ca1 O5B 76.8(2) . 1_455 ?
O3B Ca1 O1W 85.9(3) . . ?
O3B Ca1 O2B 72.8(2) . . ?
O3B Ca1 H2WA 60.9 . . ?
O3B Ca1 H2WB 93.3 . . ?
O3B Ca1 O3A 151.3(2) . . ?
O3B Ca1 O4A 143.8(2) . . ?
O3B Ca1 O5B 81.1(2) . 1_455 ?
O4A Ca1 O2B 72.42(19) . . ?
O4A Ca1 H2WA 133.3 . . ?
O4A Ca1 H2WB 107.7 . . ?
O4A Ca1 O5B 129.7(2) . 1_455 ?
O4B Ca1 O1W 148.6(3) 1_455 . ?
O4B Ca1 O2B 76.1(2) 1_455 . ?
O4B Ca1 H2WA 140.9 1_455 . ?
O4B Ca1 H2WB 142.4 1_455 . ?
O4B Ca1 O3A 89.5(2) 1_455 . ?
O4B Ca1 O3B 97.1(2) 1_455 . ?
O4B Ca1 O4A 84.1(2) 1_455 . ?
O4B Ca1 O5B 63.8(2) 1_455 1_455 ?
O5B Ca1 H2WA 80.2 1_455 . ?
O5B Ca1 H2WB 82.4 1_455 . ?
C5A O1A C1A 111.5(6) . . ?
C1B O1B C4B 110.9(7) . . ?
Ca1 O1W H1WA 116.9 . . ?
Ca1 O1W H1WB 137.6 . . ?
H1WA O1W H1WB 102.2 . . ?
C1A O2A H2A 109.5 . . ?
Ca1 O2B H2B 106.3 . . ?
C1B O2B Ca1 131.5(5) . . ?
C1B O2B H2B 109.5 . . ?
Ca1 O2W H2WA 109.4 . . ?
Ca1 O2W H2WB 95.3 . . ?
H2WA O2W H2WB 126.2 . . ?
Ca1 O3A H3A 126.7 . . ?
C3A O3A Ca1 120.3(5) . . ?
C3A O3A H3A 109.5 . . ?
Ca1 O3B H3B 118.1 . . ?
C3B O3B Ca1 132.2(5) . . ?
C3B O3B H3B 109.5 . . ?
Ca1 O4A H4A 120.4 . . ?
C4A O4A Ca1 119.5(4) . . ?
C4A O4A H4A 109.5 . . ?
Ca1 O4B H4B 125.1 1_655 . ?
C5B O4B Ca1 123.9(5) . 1_655 ?
C5B O4B H4B 109.5 . . ?
C6A O5A H5A 109.5 . . ?
Ca1 O5B H5B 111.9 1_655 . ?
C6B O5B Ca1 117.2(6) . 1_655 ?
C6B O5B H5B 109.5 . . ?
O1A C1A H1A 108.3 . . ?
O1A C1A C2A 109.3(6) . . ?
O2A C1A O1A 108.2(7) . . ?
O2A C1A H1A 108.3 . . ?
O2A C1A C2A 114.2(7) . . ?
C2A C1A H1A 108.3 . . ?
O1B C1B O2B 111.1(8) . . ?
O1B C1B H1B 110.3 . . ?
O1B C1B C2B 106.2(8) . . ?
O2B C1B H1B 110.3 . . ?
O2B C1B C2B 108.6(8) . . ?
C2B C1B H1B 110.3 . . ?
C1A C2A H2AA 109.4 . . ?
C1A C2A H2AB 109.4 . . ?
H2AA C2A H2AB 108.0 . . ?
C3A C2A C1A 111.2(7) . . ?
C3A C2A H2AA 109.4 . . ?
C3A C2A H2AB 109.4 . . ?
C1B C2B H2BA 111.4 . . ?
C1B C2B H2BB 111.4 . . ?
C1B C2B C3B 101.9(7) . . ?
H2BA C2B H2BB 109.2 . . ?
C3B C2B H2BA 111.4 . . ?
C3B C2B H2BB 111.4 . . ?
O3A C3A C2A 110.6(7) . . ?
O3A C3A H3AA 109.0 . . ?
O3A C3A C4A 107.0(6) . . ?
C2A C3A H3AA 109.0 . . ?
C2A C3A C4A 112.3(7) . . ?
C4A C3A H3AA 109.0 . . ?
O3B C3B C2B 109.6(7) . . ?
O3B C3B H3BA 110.4 . . ?
O3B C3B C4B 112.3(6) . . ?
C2B C3B H3BA 110.4 . . ?
C2B C3B C4B 103.5(7) . . ?
C4B C3B H3BA 110.4 . . ?
O4A C4A C3A 108.6(7) . . ?
O4A C4A H4AA 108.7 . . ?
O4A C4A C5A 113.4(7) . . ?
C3A C4A H4AA 108.7 . . ?
C3A C4A C5A 108.7(6) . . ?
C5A C4A H4AA 108.7 . . ?
O1B C4B C3B 104.2(7) . . ?
O1B C4B H4BA 110.2 . . ?
O1B C4B C5B 107.7(7) . . ?
C3B C4B H4BA 110.2 . . ?
C5B C4B C3B 114.2(7) . . ?
C5B C4B H4BA 110.2 . . ?
O1A C5A C4A 110.8(6) . . ?
O1A C5A H5AA 108.0 . . ?
O1A C5A C6A 108.3(7) . . ?
C4A C5A H5AA 108.0 . . ?
C6A C5A C4A 113.5(7) . . ?
C6A C5A H5AA 108.0 . . ?
O4B C5B C4B 110.1(7) . . ?
O4B C5B H5BA 109.1 . . ?
O4B C5B C6B 106.4(7) . . ?
C4B C5B H5BA 109.1 . . ?
C6B C5B C4B 113.0(7) . . ?
C6B C5B H5BA 109.1 . . ?
O5A C6A C5A 108.6(7) . . ?
O5A C6A H6AA 110.0 . . ?
O5A C6A H6AB 110.0 . . ?
C5A C6A H6AA 110.0 . . ?
C5A C6A H6AB 110.0 . . ?
H6AA C6A H6AB 108.3 . . ?
O5B C6B C5B 107.9(7) . . ?
O5B C6B H6BA 110.1 . . ?
O5B C6B H6BB 110.1 . . ?
C5B C6B H6BA 110.1 . . ?
C5B C6B H6BB 110.1 . . ?
H6BA C6B H6BB 108.4 . . ?
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
Ca1 O1W 2.447(8) . ?
Ca1 O2B 2.478(6) . ?
Ca1 O2W 2.388(7) . ?
Ca1 H2WA 2.7884 . ?
Ca1 H2WB 2.6073 . ?
Ca1 O3A 2.468(6) . ?
Ca1 O3B 2.429(6) . ?
Ca1 O4A 2.471(5) . ?
Ca1 O4B 2.415(6) 1_455 ?
Ca1 O5B 2.500(7) 1_455 ?
O1A C1A 1.434(10) . ?
O1A C5A 1.433(10) . ?
O1B C1B 1.394(13) . ?
O1B C4B 1.453(11) . ?
O1W H1WA 0.8502 . ?
O1W H1WB 0.8500 . ?
O2A H2A 0.8200 . ?
O2A C1A 1.387(11) . ?
O2B H2B 0.8200 . ?
O2B C1B 1.427(11) . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8500 . ?
O3A H3A 0.8200 . ?
O3A C3A 1.429(9) . ?
O3B H3B 0.8200 . ?
O3B C3B 1.418(10) . ?
O4A H4A 0.8200 . ?
O4A C4A 1.427(10) . ?
O4B H4B 0.8200 . ?
O4B C5B 1.437(11) . ?
O5A H5A 0.8200 . ?
O5A C6A 1.427(11) . ?
O5B H5B 0.8200 . ?
O5B C6B 1.416(11) . ?
C1A H1A 0.9800 . ?
C1A C2A 1.520(11) . ?
C1B H1B 0.9800 . ?
C1B C2B 1.500(14) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A C3A 1.509(13) . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
C2B C3B 1.506(12) . ?
C3A H3AA 0.9800 . ?
C3A C4A 1.516(11) . ?
C3B H3BA 0.9800 . ?
C3B C4B 1.536(12) . ?
C4A H4AA 0.9800 . ?
C4A C5A 1.527(11) . ?
C4B H4BA 0.9800 . ?
C4B C5B 1.518(12) . ?
C5A H5AA 0.9800 . ?
C5A C6A 1.511(11) . ?
C5B H5BA 0.9800 . ?
C5B C6B 1.514(14) . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6B H6BA 0.9700 . ?
C6B H6BB 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1W H1WA I1 0.85 2.90 3.714(9) 159.8 . yes
O1W H1WB I2 0.85 3.27 3.930(8) 136.2 . yes
O1W H1WB O5A 0.85 2.47 3.240(12) 150.5 2_646 yes
O2A H2A I2 0.82 2.65 3.460(7) 168.9 . yes
O2B H2B I1 0.82 2.65 3.463(6) 174.2 . yes
O2W H2WA O1A 0.85 2.05 2.829(9) 151.9 2_646 yes
O2W H2WA O2A 0.85 2.76 3.416(10) 134.9 2_646 yes
O3A H3A O5A 0.82 2.09 2.828(9) 148.9 2_546 yes
O3B H3B O2A 0.82 1.96 2.764(8) 165.7 2_646 yes
O4A H4A I1 0.82 2.84 3.535(6) 143.9 . yes
O4B H4B I2 0.82 2.80 3.585(6) 160.1 1_656 yes
O5A H5A I2 0.82 2.68 3.489(7) 169.1 2_656 yes
O5B H5B I2 0.82 2.78 3.560(6) 158.6 2_746 yes
C1B H1B O2A 0.98 2.72 3.640(11) 156.0 1_656 yes
C2B H2BA O4B 0.97 2.97 3.763(12) 140.1 1_455 yes
C2B H2BB I1 0.97 3.30 3.977(9) 128.9 2_747 yes
C3A H3AA O1W 0.98 2.97 3.759(12) 138.7 1_455 yes
C3B H3BA I1 0.98 3.15 3.937(8) 138.5 2_747 yes
C4B H4BA O3A 0.98 2.90 3.678(11) 136.5 1_655 yes
C6A H6AA I1 0.97 3.25 3.881(10) 124.4 1_455 yes
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 O2B C1B O1B 77.9(9) . . . . ?
Ca1 O2B C1B C2B -38.5(10) . . . . ?
Ca1 O3A C3A C2A 82.8(7) . . . . ?
Ca1 O3A C3A C4A -39.8(8) . . . . ?
Ca1 O3B C3B C2B 38.7(10) . . . . ?
Ca1 O3B C3B C4B -75.8(9) . . . . ?
Ca1 O4A C4A C3A -39.6(8) . . . . ?
Ca1 O4A C4A C5A -160.5(5) . . . . ?
Ca1 O4B C5B C4B -90.9(8) 1_655 . . . ?
Ca1 O4B C5B C6B 31.8(8) 1_655 . . . ?
Ca1 O5B C6B C5B 46.6(9) 1_655 . . . ?
O1A C1A C2A C3A 55.4(9) . . . . ?
O1A C5A C6A O5A 64.6(9) . . . . ?
O1B C1B C2B C3B -34.9(9) . . . . ?
O1B C4B C5B O4B -51.5(9) . . . . ?
O1B C4B C5B C6B -170.3(7) . . . . ?
O2A C1A C2A C3A 176.7(7) . . . . ?
O2B C1B C2B C3B 84.6(8) . . . . ?
O3A C3A C4A O4A 48.5(9) . . . . ?
O3A C3A C4A C5A 172.3(7) . . . . ?
O3B C3B C4B O1B 95.5(8) . . . . ?
O3B C3B C4B C5B -147.2(7) . . . . ?
O4A C4A C5A O1A 64.3(8) . . . . ?
O4A C4A C5A C6A -57.8(10) . . . . ?
O4B C5B C6B O5B -47.7(9) . . . . ?
C1A O1A C5A C4A 64.3(8) . . . . ?
C1A O1A C5A C6A -170.6(6) . . . . ?
C1A C2A C3A O3A -170.7(7) . . . . ?
C1A C2A C3A C4A -51.3(9) . . . . ?
C1B O1B C4B C3B 1.0(10) . . . . ?
C1B O1B C4B C5B -120.7(8) . . . . ?
C1B C2B C3B O3B -85.6(8) . . . . ?
C1B C2B C3B C4B 34.5(8) . . . . ?
C2A C3A C4A O4A -73.0(8) . . . . ?
C2A C3A C4A C5A 50.8(9) . . . . ?
C2B C3B C4B O1B -22.6(8) . . . . ?
C2B C3B C4B C5B 94.6(8) . . . . ?
C3A C4A C5A O1A -56.5(9) . . . . ?
C3A C4A C5A C6A -178.6(7) . . . . ?
C3B C4B C5B O4B -166.7(6) . . . . ?
C3B C4B C5B C6B 74.5(9) . . . . ?
C4A C5A C6A O5A -171.9(8) . . . . ?
C4B O1B C1B O2B -96.4(9) . . . . ?
C4B O1B C1B C2B 21.4(10) . . . . ?
C4B C5B C6B O5B 73.2(10) . . . . ?
C5A O1A C1A O2A 172.6(6) . . . . ?
C5A O1A C1A C2A -62.5(9) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0028 6.9979 5.0052 -1.0016 0.2713 -0.2373
4.0015 5.0012 0.0009 -0.3635 0.0950 -0.9349
-1.0035 3.9983 6.0044 -0.8398 0.4703 0.0521
-3.0005 -6.0001 -1.0021 0.5462 -0.0801 0.7765
-0.0008 8.9966 0.0046 -0.7751 -0.4813 -0.2947
-3.0026 7.9948 1.0056 -0.8191 -0.5705 0.3148
-0.0017 -5.9972 4.9986 0.1180 0.9665 0.1884
-0.9988 5.9965 -4.9982 -0.1348 -1.0571 0.0044
1.0003 -7.9960 1.9962 0.5463 0.7767 0.0660
-4.0013 2.9956 -1.9975 -0.1660 -0.7811 0.6761
3.0004 -2.9963 2.9982 0.0695 0.8196 -0.4849
4.0044 -2.9963 -5.0048 0.7242 -0.1228 -0.6648
-1.9990 -6.9992 -3.0037 0.8086 -0.1942 0.6196
0.0028 -6.9979 -5.0052 1.0016 -0.2713 0.2373

_cod_database_fobs_code 2108834
