Modulating the hydration behaviour of calcium chloride by lactam complexation.
Perrin, Andrea; Musa, Osama M.; Steed, Jonathan W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12181–12187; doi:10.1039/c6dt02296k

data_7039863
_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       '\w 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/[\s^2^(Fo^2^)+(0.0395P)^2^+0.7921P] where P=(Fo^2^+2Fc^2^)/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)
;