One water to bind a chloride-chloride ion pair: isolation of discrete [Cl<sub>2</sub>(H<sub>2</sub>O)]<sup>2-</sup> in the solid state.
Curnow, Owen J.; Senthooran, Rathiga; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9579–9582; doi:10.1039/d0dt02300k

data_7704745
_publ_section_title
;
 One water to bind a chloride-chloride ion pair: isolation of discrete
 [Cl<sub>2</sub>(H<sub>2</sub>O)]<sup>2-</sup> in the solid state.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9579
_journal_page_last               9582
_journal_paper_doi               10.1039/d0dt02300k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(Cl), 2(C23 H34 F12 N3), H2 O'
_chemical_formula_sum            'C46 H70 Cl2 F24 N6 O'
_chemical_formula_weight         1249.98
_chemical_name_systematic
'bis(bis(2,2,2-trifluoroethyl)amino)dihexylaminocyclopropenium chloride semihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-04 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.999(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6228(4)
_cell_length_b                   38.0161(17)
_cell_length_c                   15.0865(5)
_cell_measurement_reflns_used    4449
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      74.8630
_cell_measurement_theta_min      4.3340
_cell_volume                     6069.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -72.00  39.00   1.00   15.50    --  -38.50  19.00   0.00  111
  2  \w      2.00  30.00   1.00   15.50    --   41.88 -99.00-180.00   28
  3  \w     30.00 113.00   1.00   15.50    --   41.88  37.00-150.00   83
  4  \w     48.00 107.00   1.00   62.00    --  111.00 -94.00-150.00   59
  5  \w     48.00  76.00   1.00   62.00    --  111.00 -61.00-150.00   28
  6  \w     79.00 131.00   1.00   62.00    --  111.00 -61.00-150.00   52
  7  \w     38.00 115.00   1.00   62.00    --  111.00 -30.00 120.00   77
  8  \w     47.00 125.00   1.00   62.00    --  111.00 -45.00 -60.00   78
  9  \w    105.00 147.00   1.00   62.00    --  111.00 111.00 -90.00   42
 10  \w     45.00 113.00   1.00   62.00    --  111.00-111.00-180.00   68
 11  \w    102.00 142.00   1.00   62.00    --  111.00 111.00-180.00   40
 12  \w     90.00 156.00   1.00   62.00    --  111.00  45.00 -30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0796436000
_diffrn_orient_matrix_UB_12      -0.0192372000
_diffrn_orient_matrix_UB_13      -0.0655551000
_diffrn_orient_matrix_UB_21      -0.0484728000
_diffrn_orient_matrix_UB_22      0.0256391000
_diffrn_orient_matrix_UB_23      -0.0743748000
_diffrn_orient_matrix_UB_31      0.1117298000
_diffrn_orient_matrix_UB_32      0.0248108000
_diffrn_orient_matrix_UB_33      0.0261013000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.499
_diffrn_reflns_theta_min         3.749
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.974
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             2584
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, diethylether, water'
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         11795
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6454
_reflns_number_total             11795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02300k2.cif
_cod_data_source_block           rse56ap
_cod_depositor_comments          'Adding full bibliography for 7704745.cif.'
_cod_database_code               7704745
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C23H34F12N3Cl
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H) groups
2. Restrained distances
 C6J2-C6K2
 1.5 with sigma of 0.02
 C6K1-C6L1
 1.5 with sigma of 0.02
 C6L2-C6K2
 1.5 with sigma of 0.02
 C6J1-C6K1
 1.5 with sigma of 0.02
 H6FA-H6EA
 2.326 with sigma of 0.02
 H6LA-H6KD
 2.326 with sigma of 0.02
 O1-H1B
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6L1) = Uanis(C6L2)
Uanis(C6K1) = Uanis(C6K2)
Uanis(C6K2) = Uanis(C6K1)
4. Others
 Sof(C6L1)=Sof(H6LD)=Sof(H6LE)=Sof(H6LF)=1-FVAR(1)
 Sof(C6L2)=Sof(H6LA)=Sof(H6LB)=Sof(H6LC)=FVAR(1)
 Fixed Sof: H6IA(0.5) H6IB(0.5) H6IC(0.5) H6ID(0.5) H3KA(0.5) H3KB(0.5)
 H3KC(0.5) H3KD(0.5) C3L2(0.5) H3LA(0.5) H3LB(0.5) H3LC(0.5) C6J2(0.5)
 H6JA(0.5) H6JB(0.5) C6J1(0.5) H6JC(0.5) H6JD(0.5) C6K1(0.5) H6KA(0.5)
 H6KB(0.5) C3L1(0.5) H3LD(0.5) H3LE(0.5) H3LF(0.5) C6K2(0.5) H6KC(0.5) H6KD(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C11(H11A,H11B), C21(H21A,H21B), C23(H23A,H23B), C3A(H3AA,
 H3AB), C3G(H3GA,H3GB), C51(H51A,H51B), C53(H53A,H53B), C3H(H3HA,H3HB),
 C41(H41A,H41B), C3B(H3BA,H3BB), C6G(H6GA,H6GB), C6A(H6AA,H6AB), C43(H43A,H43B),
  C3I(H3IA,H3IB), C3C(H3CA,H3CB), C6B(H6BA,H6BB), C6I(H6IA,H6IB), C6I(H6IC,
 H6ID), C3J(H3JA,H3JB), C6C(H6CA,H6CB), C6H(H6HA,H6HB), C3D(H3DA,H3DB),
 C6D(H6DA,H6DB), C3E(H3EA,H3EB), C3K(H3KA,H3KB), C3K(H3KC,H3KD), C6E(H6EA,H6EB),
  C6J2(H6JA,H6JB), C6J1(H6JC,H6JD), C6K1(H6KA,H6KB), C6K2(H6KC,H6KD)
5.b Idealised Me refined as rotating group:
 C3F(H3FA,H3FB,H3FC), C6F(H6FA,H6FB,H6FC), C3L2(H3LA,H3LB,H3LC), C6L2(H6LA,
 H6LB,H6LC), C3L1(H3LD,H3LE,H3LF), C6L1(H6LD,H6LE,H6LF)
;
_shelx_res_checksum              21373
_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 3.121
_oxdiff_exptl_absorpt_empirical_full_min 0.587