#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:43:31 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185326 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/98/7039863.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_7039863
loop_
_publ_author_name
'Perrin, Andrea'
'Musa, Osama M.'
'Steed, Jonathan W.'
_publ_section_title
;
 Modulating the hydration behaviour of calcium chloride by lactam
 complexation.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12181
_journal_page_last               12187
_journal_paper_doi               10.1039/c6dt02296k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C12 H30 Ca N2 O8, 2(Cl), H2 O'
_chemical_formula_sum            'C12 H32 Ca Cl2 N2 O9'
_chemical_formula_weight         459.38
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2016-07-05 deposited with the CCDC.
2016-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                99.325(5)
_cell_angle_beta                 95.103(4)
_cell_angle_gamma                104.163(5)
_cell_formula_units_Z            2
_cell_length_a                   8.8007(5)
_cell_length_b                   8.9311(5)
_cell_length_c                   14.7500(8)
_cell_measurement_reflns_used    3965
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.4757
_cell_measurement_theta_min      2.6181
_cell_volume                     1099.19(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -91.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429    0.0000 -120.0000 133

  2 omega -100.00  -66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429 -179.0000    0.0000 34

  3 omega  -95.00  -14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -38.0000   30.0000 81

  4 omega -100.00  -41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429 -179.0000  150.0000 59

  5 omega   56.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000   30.0000 25

  6 omega   23.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -122.0000   34.0000 56

  7 omega   20.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -122.0000 -145.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0049377000
_diffrn_orient_matrix_UB_12      0.0786415000
_diffrn_orient_matrix_UB_13      0.0122795000
_diffrn_orient_matrix_UB_21      -0.0034995000
_diffrn_orient_matrix_UB_22      0.0069688000
_diffrn_orient_matrix_UB_23      -0.0473168000
_diffrn_orient_matrix_UB_31      -0.0836655000
_diffrn_orient_matrix_UB_32      -0.0269840000
_diffrn_orient_matrix_UB_33      -0.0053728000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8493
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4521
_exptl_crystal_size_mid          0.3035
_exptl_crystal_size_min          0.1295
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+0.7921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3745
_reflns_number_total             4306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt02296k2.cif
_cod_data_source_block           ap82_2
_cod_depositor_comments
'Adding full bibliography for 7039860--7039863.cif.'
_cod_original_cell_volume        1099.18(11)
_cod_database_code               7039863
_chemical_oxdiff_formula         CaCl2C12H32O9N2
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O6S(H6SA,H6SB)
2.b Rotating group:
 O1S(H1SA,H1SB), O4S(H4SA,H4SB), O5S(H5SA,H5SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB)
2.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C8(H8A,H8B), C7(H7A,H7B), C2(H2A,H2B), C4(H4A,H4B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C3(H3A,H3B)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_posn
Ca1 Ca 0.12529(5) 0.18038(5) 0.29170(3) 0.01196(12) Uani 1 1 d .
Cl1 Cl 0.11631(6) 0.71216(6) 0.41166(4) 0.01842(13) Uani 1 1 d .
O1S O 0.07608(18) 0.35734(18) 0.41852(10) 0.0198(3) Uani 1 1 d .
H1SA H 0.0302 0.3291 0.4684 0.030 Uiso 1 1 d GR
H1SB H 0.1001 0.4640 0.4248 0.030 Uiso 1 1 d GR
O4S O 0.11292(18) 0.12901(18) 0.12499(10) 0.0185(3) Uani 1 1 d .
H4SA H 0.1483 0.0541 0.0917 0.028 Uiso 1 1 d GR
H4SB H 0.0722 0.1818 0.0864 0.028 Uiso 1 1 d GR
O1 O 0.40281(17) 0.25182(18) 0.30244(11) 0.0188(3) Uani 1 1 d .
O2 O 0.64930(16) 0.74651(17) 0.39277(10) 0.0158(3) Uani 1 1 d .
O5S O 0.1671(2) 0.43654(19) 0.24858(11) 0.0239(4) Uani 1 1 d .
H5SA H 0.1096 0.4913 0.2784 0.036 Uiso 1 1 d GR
H5SB H 0.1394 0.4256 0.1884 0.036 Uiso 1 1 d GR
O2S O 0.1498(2) 0.07656(19) 0.43426(11) 0.0238(4) Uani 1 1 d .
H2SA H 0.0674 -0.0016 0.4338 0.036 Uiso 1 1 d GR
H2SB H 0.1556 0.1506 0.4822 0.036 Uiso 1 1 d GR
N1 N 0.6361(2) 0.4257(2) 0.29330(12) 0.0157(4) Uani 1 1 d .
O6S O 0.2158(2) 0.4866(2) 0.07371(12) 0.0254(4) Uani 1 1 d .
H6SA H 0.2031 0.5770 0.0648 0.038 Uiso 1 1 d G
H6SB H 0.1409 0.4113 0.0393 0.038 Uiso 1 1 d G
N2 N 0.6094(2) 0.9374(2) 0.25846(12) 0.0173(4) Uani 1 1 d .
O3S O 0.1034(2) -0.09704(19) 0.24893(11) 0.0307(4) Uani 1 1 d .
H3SA H 0.1001 -0.1618 0.2875 0.046 Uiso 1 1 d GR
H3SB H 0.0974 -0.1481 0.1925 0.046 Uiso 1 1 d GR
O3 O 0.85094(18) 1.1048(2) 0.26196(12) 0.0269(4) Uani 1 1 d .
C6 C 0.5908(3) 0.6050(3) 0.42728(15) 0.0171(4) Uani 1 1 d .
H6A H 0.4762 0.5619 0.4058 0.021 Uiso 1 1 calc R
H6B H 0.6065 0.6282 0.4959 0.021 Uiso 1 1 calc R
C1 C 0.5044(2) 0.3148(3) 0.25638(15) 0.0151(4) Uani 1 1 d .
C5 C 0.6785(2) 0.4857(3) 0.39254(15) 0.0168(4) Uani 1 1 d .
H5A H 0.7937 0.5353 0.4061 0.020 Uiso 1 1 calc R
H5B H 0.6539 0.3970 0.4260 0.020 Uiso 1 1 calc R
C9 C 0.7369(2) 0.9982(3) 0.22024(15) 0.0187(5) Uani 1 1 d .
C8 C 0.5968(3) 0.9830(3) 0.35623(15) 0.0213(5) Uani 1 1 d .
H8A H 0.5215 1.0491 0.3626 0.026 Uiso 1 1 calc R
H8B H 0.7013 1.0470 0.3890 0.026 Uiso 1 1 calc R
C7 C 0.5415(3) 0.8425(3) 0.40104(16) 0.0213(5) Uani 1 1 d .
H7A H 0.5349 0.8784 0.4673 0.026 Uiso 1 1 calc R
H7B H 0.4347 0.7806 0.3706 0.026 Uiso 1 1 calc R
C2 C 0.5012(3) 0.2786(3) 0.15309(16) 0.0233(5) Uani 1 1 d .
H2A H 0.4043 0.2944 0.1211 0.028 Uiso 1 1 calc R
H2B H 0.5046 0.1685 0.1323 0.028 Uiso 1 1 calc R
C4 C 0.7396(3) 0.4769(3) 0.22557(16) 0.0256(5) Uani 1 1 d .
H4A H 0.8403 0.4473 0.2353 0.031 Uiso 1 1 calc R
H4B H 0.7632 0.5922 0.2300 0.031 Uiso 1 1 calc R
C10 C 0.7162(3) 0.9177(3) 0.12037(16) 0.0274(6) Uani 1 1 d .
H10A H 0.7877 0.8481 0.1113 0.033 Uiso 1 1 calc R
H10B H 0.7384 0.9959 0.0795 0.033 Uiso 1 1 calc R
C11 C 0.5430(3) 0.8221(3) 0.10002(16) 0.0280(6) Uani 1 1 d .
H11A H 0.5332 0.7159 0.0638 0.034 Uiso 1 1 calc R
H11B H 0.4787 0.8755 0.0647 0.034 Uiso 1 1 calc R
C12 C 0.4892(3) 0.8116(3) 0.19554(16) 0.0250(5) Uani 1 1 d .
H12A H 0.3828 0.8295 0.1974 0.030 Uiso 1 1 calc R
H12B H 0.4873 0.7077 0.2115 0.030 Uiso 1 1 calc R
C3 C 0.6465(3) 0.3918(4) 0.13318(18) 0.0393(7) Uani 1 1 d .
H3A H 0.7103 0.3342 0.0964 0.047 Uiso 1 1 calc R
H3B H 0.6160 0.4675 0.0977 0.047 Uiso 1 1 calc R
Cl2 Cl 0.09360(7) 0.77948(7) 0.03605(4) 0.02338(14) Uani 1 1 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'
Ca Ca 0.2262 0.3064 '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
_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
-12 -2 3 0.2031 -11.9921 -1.9989 2.9909 -0.0613 -0.1135 1.0412
12 2 -3 0.2031 11.9921 1.9989 -2.9909 0.0613 0.1135 -1.0412
-1 6 -20 0.0919 -1.0012 5.9966 -19.9694 0.2313 0.9902 0.0292
1 -6 20 0.1083 1.0012 -5.9966 19.9694 -0.2313 -0.9902 -0.0292
1 7 15 0.0617 0.9935 6.9963 14.9744 0.7292 -0.6633 -0.3524
-7 6 15 0.0835 -7.0012 5.9968 14.9715 0.6900 -0.6421 0.3435
2 -7 -16 0.0558 2.0048 -6.9963 -15.9716 -0.7562 0.7000 0.1069
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
O1S Ca1 O4S 142.76(6) . .
O1S Ca1 O5S 72.41(5) . .
O1S Ca1 O2S 70.17(5) . .
O1S Ca1 O3S 138.01(6) . .
O4S Ca1 O5S 75.00(5) . .
O4S Ca1 O2S 146.36(6) . .
O1 Ca1 O1S 103.00(6) . .
O1 Ca1 O4S 88.54(5) . .
O1 Ca1 O5S 80.17(6) . .
O1 Ca1 O2S 88.66(6) . .
O1 Ca1 O3S 93.76(6) . .
O5S Ca1 O2S 137.21(6) . .
O3S Ca1 O4S 74.67(6) . .
O3S Ca1 O5S 149.19(6) . .
O3S Ca1 O2S 72.08(6) . .
O3 Ca1 O1S 82.52(6) 1_445 .
O3 Ca1 O4S 84.60(6) 1_445 .
O3 Ca1 O1 173.13(6) 1_445 .
O3 Ca1 O5S 97.87(6) 1_445 .
O3 Ca1 O2S 97.13(6) 1_445 .
O3 Ca1 O3S 84.56(6) 1_445 .
C1 O1 Ca1 136.98(14) . .
C7 O2 C6 110.49(16) . .
C1 N1 C5 123.38(17) . .
C1 N1 C4 114.00(18) . .
C5 N1 C4 122.54(18) . .
C9 N2 C8 122.77(19) . .
C9 N2 C12 114.29(19) . .
C8 N2 C12 122.74(18) . .
C9 O3 Ca1 143.37(16) . 1_665
O2 C6 C5 109.31(16) . .
O1 C1 N1 124.1(2) . .
O1 C1 C2 126.85(19) . .
N1 C1 C2 109.04(18) . .
N1 C5 C6 111.98(17) . .
N2 C9 C10 109.13(19) . .
O3 C9 N2 124.0(2) . .
O3 C9 C10 126.8(2) . .
N2 C8 C7 112.19(19) . .
O2 C7 C8 109.79(17) . .
C1 C2 C3 105.37(19) . .
N1 C4 C3 104.30(18) . .
C9 C10 C11 104.71(19) . .
C10 C11 C12 105.13(18) . .
N2 C12 C11 103.37(18) . .
C4 C3 C2 106.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1S 2.3886(16) .
Ca1 O4S 2.4148(15) .
Ca1 O1 2.3523(15) .
Ca1 O5S 2.4239(16) .
Ca1 O2S 2.4447(16) .
Ca1 O3S 2.4108(17) .
Ca1 O3 2.3229(16) 1_445
O1 C1 1.250(3) .
O2 C6 1.435(3) .
O2 C7 1.427(3) .
N1 C1 1.332(3) .
N1 C5 1.456(3) .
N1 C4 1.464(3) .
N2 C9 1.336(3) .
N2 C8 1.455(3) .
N2 C12 1.466(3) .
O3 Ca1 2.3229(16) 1_665
O3 C9 1.235(3) .
C6 C5 1.512(3) .
C1 C2 1.502(3) .
C9 C10 1.505(3) .
C8 C7 1.509(3) .
C2 C3 1.507(3) .
C4 C3 1.506(3) .
C10 C11 1.530(3) .
C11 C12 1.535(3) .
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
O5S H5SB O6S 0.88 1.98 2.741(2) 143.2
