Piperazine linked salicylaldoxime and salicylaldimine-based dicopper(ii) receptors for anions.
De Silva, D Nirosha T; Jameson, Geoffrey B.; Pannu, Ajay Pal Singh; Pouhet, Raphëlle; Wenzel, Marco; Plieger, Paul G.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15949–15959; doi:10.1039/c5dt02551f

data_7036152
_publ_section_title
;
 Piperazine linked salicylaldoxime and salicylaldimine-based dicopper(ii)
 receptors for anions.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15949
_journal_page_last               15959
_journal_paper_doi               10.1039/c5dt02551f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'2(C80 H96 Cu2 N8 O4), 6(B F4), C2 H6 B2 F5 O2, C2 H6 B2 F3 O2, 0.5(O)'
_chemical_formula_sum            'C164 H204 B10 Cu4 F32 N16 O12.5'
_chemical_formula_weight         3569.68
_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     iterative
_audit_creation_date             2015-08-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-08-07 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                93.011(7)
_cell_angle_beta                 100.424(7)
_cell_angle_gamma                101.741(7)
_cell_formula_units_Z            1
_cell_length_a                   13.8450(3)
_cell_length_b                   16.2809(3)
_cell_length_c                   20.9717(15)
_cell_measurement_reflns_used    29055
_cell_measurement_temperature    143
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_cell_volume                     4532.3(4)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      143
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
scan:
    Number of images: 45
               Slice: 20.0000 - 200.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 45
               Slice: 20.0000 - 200.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 45
               Slice: 20.0000 - 200.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 43
               Slice: 22.0000 - 197.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 42
               Slice: 22.0000 - 192.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 41
               Slice: 20.0000 - 185.0000
         Image width: 4.0000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type  'Rigaku RAXIS conversion'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.070722
_diffrn_orient_matrix_UB_12      -0.011238
_diffrn_orient_matrix_UB_13      0.007306
_diffrn_orient_matrix_UB_21      -0.019835
_diffrn_orient_matrix_UB_22      0.031861
_diffrn_orient_matrix_UB_23      -0.037945
_diffrn_orient_matrix_UB_31      -0.016267
_diffrn_orient_matrix_UB_32      -0.053182
_diffrn_orient_matrix_UB_33      -0.029629
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59339
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         6.586
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   FS_Process
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1165
_refine_ls_number_reflns         14809
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.522
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0929
_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^)+(0.1937P)^2^+3.1050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2686
_refine_ls_wR_factor_ref         0.2942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10753
_reflns_number_total             14809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02551f2.cif
_cod_data_source_block           1042539cmplex3
_cod_depositor_comments
'Adding full bibliography for 7036149--7036153.cif.'
_cod_original_formula_sum        'C164 H204 B10 Cu4 F32 N16 O12.50'
_cod_database_code               7036152
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F11 = B1-F12 = B1-F13 = B1-F14 = B2-F21 = B2-F22 = B2-F23 = B2-F24 = B3-
 F31 = B3-F32 = B3-F33 = B3-F34 = B4-F41 = B4-F42 = B4-F43 = B1A-F11A = B1A-
 F12A = B1A-F13A = B1A-F14A = B2A-F21A = B2A-F22A = B2A-F23A = B2A-F24A = B4A-
 F41A = B4A-F42A = B4A-F41A
 1.29749 with sigma of 0.02
 F11-F12 = F11-F13 = F11-F14 = F12-F13 = F12-F14 = F13-F14
 2.118801 with sigma of 0.02
 F21-F22 = F21-F23 = F21-F24 = F22-F23 = F22-F24 = F23-F24
 2.118801 with sigma of 0.02
 F31-F32 = F31-F33 = F31-F34 = F32-F33 = F32-F34 = F33-F34
 2.118801 with sigma of 0.02
 F41-F42 = F41-F43 = F42-F43
 2.118801 with sigma of 0.02
 F11A-F12A = F11A-F13A = F11A-F14A = F12A-F13A = F12A-F14A = F13A-F14A
 2.118801 with sigma of 0.02
 F21A-F22A = F21A-F23A = F21A-F24A = F22A-F23A = F22A-F24A = F23A-F24A
 2.118801 with sigma of 0.02
 F41A-F42A = F41A-F41A = F42A-F41A
 2.118801 with sigma of 0.02
3. Rigid bond restraints
 F11, F12, F13, F14, F11A, F12A, F13A, F14A, F21, F22, F23, F24, F21A, F22A,
 F23A, F24A, F31, F32, F33, F34, F41, F42, F43, F41A, F42A, B1, B1A, B2, B2A,
 B3, B4, B4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F11 \\sim F12 \\sim F13 \\sim F14 \\sim F11A \\sim F12A \\sim F13A \\sim F14A
\\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F21A \\sim F22A \\sim F23A \\sim
F24A \\sim F31 \\sim F32 \\sim F33 \\sim F34 \\sim F41 \\sim F42 \\sim F43
\\sim F41A \\sim F42A \\sim B1 \\sim B1A \\sim B2 \\sim B2A \\sim B3 \\sim B4
\\sim B4A \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O44 \\sim O44A \\sim
O1W: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F11 \\sim F12 \\sim F13 \\sim F14 \\sim F11A \\sim F12A \\sim F13A \\sim F14A
\\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F21A \\sim F22A \\sim F23A \\sim
F24A \\sim F31 \\sim F32 \\sim F33 \\sim F34 \\sim F41 \\sim F42 \\sim F43
\\sim F41A \\sim F42A \\sim B1 \\sim B1A \\sim B2 \\sim B2A \\sim B3 \\sim B4
\\sim B4A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O44) \\sim Ueq, Uanis(O44A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C423) \\sim Ueq, Uanis(C422) \\sim Ueq, Uanis(C424) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(B1) = Uanis(B1A)
Uanis(B4) = Uanis(B4A)
Uanis(O44) = Uanis(O44A)
5. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Sof(B1A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=1-FVAR(2)
 Sof(B1)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=FVAR(2)
 Sof(B2A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3)
 Sof(B2)=Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
 Fixed Sof: F41(0.5) F42A(0.5) O1W(0.25)
6.a Ternary CH refined with riding coordinates:
 N612(H612), N622(H622), N632(H632), N642(H642)
6.b Secondary CH2 refined with riding coordinates:
 C611(H61A,H61B), C613(H61C,H61D), C614(H61E,H61F), C621(H62A,H62B), C623(H62C,
 H62D), C624(H62E,H62F), C631(H63A,H63B), C633(H63C,H63D), C634(H63E,H63F),
 C641(H64A,H64B), C643(H64C,H64D), C644(H64E,H64F)
6.c Me refined with riding coordinates:
 C412(H41A,H41B,H41C), C413(H41D,H41E,H41F), C414(H41G,H41H,H41I), C422(H42A,
 H42B,H42C), C423(H42D,H42E,H42F), C424(H42G,H42H,H42I), C432(H43A,H43B,H43C),
 C433(H43D,H43E,H43F), C434(H43G,H43H,H43I), C442(H44A,H44B,H44C), C443(H44D,
 H44E,H44F), C444(H44G,H44H,H44I), C45(H45A,H45B,H45C), C45A(H45D,H45E,H45F)
6.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C51(H51), C52(H52), C53(H53),
 C54(H54), C211(H211), C214(H214), C215(H215), C216(H216), C217(H217),
 C218(H218), C221(H221), C224(H224), C225(H225), C226(H226), C227(H227),
 C228(H228), C231(H231), C234(H234), C235(H235), C236(H236), C237(H237),
 C238(H238), C241(H241), C244(H244), C245(H245), C246(H246), C247(H247),
 C248(H248)
;
_shelx_res_checksum              55071
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'