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_7036149
_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         'C56 H78 Cu2 N8 O8, 1(B F4), 2(C3 H7 N O)'
_chemical_formula_sum            'C62 H92 B Cu2 F4 N10 O10'
_chemical_formula_weight         1351.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-30
_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                90
_cell_angle_beta                 107.834(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0641(4)
_cell_length_b                   21.0442(5)
_cell_length_c                   22.9542(16)
_cell_measurement_reflns_used    14604
_cell_measurement_temperature    123
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_cell_volume                     7386.9(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 51
               Slice: 20.0000 - 200.0000
         Image width: 3.5000
            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: 23.0000 - 170.0000
         Image width: 3.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 47
               Slice: 20.0000 - 185.0000
         Image width: 3.5000
            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: 48
               Slice: 22.0000 - 192.0000
         Image width: 3.5000
            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: 48
               Slice: 24.0000 - 194.0000
         Image width: 3.5000
            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 Loop
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.064116
_diffrn_orient_matrix_UB_12      0.004801
_diffrn_orient_matrix_UB_13      0.006391
_diffrn_orient_matrix_UB_21      0.000575
_diffrn_orient_matrix_UB_22      -0.041799
_diffrn_orient_matrix_UB_23      -0.020595
_diffrn_orient_matrix_UB_31      -0.012848
_diffrn_orient_matrix_UB_32      0.022087
_diffrn_orient_matrix_UB_33      -0.040365
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65462
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         72.064
_diffrn_reflns_theta_min         6.628
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   FS_Process
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       Chip
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         8961
_refine_ls_number_restraints     1141
_refine_ls_restrained_S_all      1.709
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0866
_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/[\s^2^(Fo^2^)+(0.1778P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2517
_refine_ls_wR_factor_ref         0.2806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5421
_reflns_number_total             8961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02551f2.cif
_cod_data_source_block           1042536_Complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7036149--7036153.cif.
;
_cod_original_cell_volume        7386.9(6)
_cod_database_code               7036149
_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, All O(H) groups
2. Restrained distances
 F13A-F12A = F13A-F14A = F13A-F11A = F12A-F14A = F12A-F11A = F14A-F11A
 2.2652 with sigma of 0.02
 F14-F11 = F14-F12 = F14-F13 = F11-F12 = F11-F13 = F12-F13
 2.2652 with sigma of 0.02
 B1A-F13A = B1A-F12A = B1A-F14A = B1A-F11A = B1-F14 = B1-F11 = B1-F12 = B1-F13
 1.38714 with sigma of 0.02
 O243-C62 = O20B-N200 = O20B-C20B
 2.68116 with sigma of 0.02
 O20B-C20A
 1.02104 with sigma of 0.02
 C102-O100 = C20A-O20A = C20B-O20B
 1.18331 with sigma of 0.02
 C100-O100 = C201-O20A = C200-O20B
 2.88125 with sigma of 0.02
 C411-C1 = C411-C2 = C411-C3 = C411-C412 = C411-C413 = C411-C414
 1.43 with sigma of 0.01
 C412-C413 = C412-C414 = C413-C414
 2.40874 with sigma of 0.02
 C1-C2 = C1-C3 = C2-C3
 2.40874 with sigma of 0.02
3. Restrained planarity
 C201, C200, N200, C20A, O20A
 with sigma of 0.01
 C201, C200, N200, C20B, O20B
 with sigma of 0.01
4. Rigid bond restraints
 B1, B1A, C12, C31, C32, C51, C53, C54, C61, C64, C411, C20A, C20B, C200, C201,
  C1, C2, C3, C11, C13, C14, C21, C22, C23, C24, C33, C34, C41, C42, C43, C44,
 C52, C62, C63, C100, C101, C102, C211, C221, C231, C241, C421, C423, C431,
 C432, C433, C434, C441, C444, C614, C621, C623, C624, C631, C633, C643, C412,
 C413, C414, C422, C424, C442, C443, C611, C613, C634, C641, C644, F11, F11A,
 F12, F12A, F13, F13A, F14, F14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C12 \\sim C31 \\sim C32 \\sim C51 \\sim C53 \\sim C54 \\sim C61 \\sim C64 \\sim
C411 \\sim C20A \\sim C20B \\sim C200 \\sim C201 \\sim C1 \\sim C2 \\sim C3
\\sim C11 \\sim C13 \\sim C14 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C33
\\sim C34 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C52 \\sim C62 \\sim C63
\\sim C100 \\sim C101 \\sim C102 \\sim C211 \\sim C221 \\sim C231 \\sim C241
\\sim C421 \\sim C423 \\sim C431 \\sim C432 \\sim C433 \\sim C434 \\sim C441
\\sim C444 \\sim C614 \\sim C621 \\sim C623 \\sim C624 \\sim C631 \\sim C633
\\sim C643 \\sim C412 \\sim C413 \\sim C414 \\sim C422 \\sim C424 \\sim C442
\\sim C443 \\sim C611 \\sim C613 \\sim C634 \\sim C641 \\sim C644 \\sim F11
\\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim
O11 \\sim O12 \\sim O13 \\sim O14 \\sim O100 \\sim O20A \\sim O20B \\sim O213
\\sim O223 \\sim O233 \\sim O243: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 1.2
Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F14A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C411) \\sim Ueq, Uanis(C20A)
\\sim Ueq, Uanis(C20B) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C201) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C211) \\sim Ueq, Uanis(C221) \\sim Ueq,
Uanis(C231) \\sim Ueq, Uanis(C241) \\sim Ueq, Uanis(C421) \\sim Ueq,
Uanis(C423) \\sim Ueq, Uanis(C431) \\sim Ueq, Uanis(C432) \\sim Ueq,
Uanis(C433) \\sim Ueq, Uanis(C434) \\sim Ueq, Uanis(C441) \\sim Ueq,
Uanis(C444) \\sim Ueq, Uanis(C614) \\sim Ueq, Uanis(C621) \\sim Ueq,
Uanis(C623) \\sim Ueq, Uanis(C624) \\sim Ueq, Uanis(C631) \\sim Ueq,
Uanis(C633) \\sim Ueq, Uanis(C643) \\sim Ueq, Uanis(C412) \\sim Ueq,
Uanis(C413) \\sim Ueq, Uanis(C414) \\sim Ueq, Uanis(C422) \\sim Ueq,
Uanis(C424) \\sim Ueq, Uanis(C442) \\sim Ueq, Uanis(C443) \\sim Ueq,
Uanis(C611) \\sim Ueq, Uanis(C613) \\sim Ueq, Uanis(C634) \\sim Ueq,
Uanis(C641) \\sim Ueq, Uanis(C644) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(B1A)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O100) \\sim Ueq, Uanis(O20A) \\sim Ueq, Uanis(O20B)
\\sim Ueq, Uanis(O213) \\sim Ueq, Uanis(O223) \\sim Ueq, Uanis(O233) \\sim Ueq,
Uanis(O243) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(4)
 Sof(C412)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C413)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C414)=Sof(H41G)=Sof(H41H)=Sof(H41I)=FVAR(4)
 1(DFIX)=1(DFIX)=1.633*FVAR(8)
 Fixed Sof: F11(0.6667) F11A(0.33333) F12(0.6667) F12A(0.33333) F13(0.6667)
 F13A(0.33333) F14(0.6667) F14A(0.33333) O20A(0.33333) C20A(0.33333)
 H20A(0.33333) O20B(0.6667) C20B(0.6667) H20B(0.6667) B1(0.6667) B1A(0.33333)
7.a Free rotating group:
 C411(O100,O20A,C20A,O20B,C20B,N200,C200,C201,O213,O223,O233,O243,N100,N212,
 N222,N232,N242,N612,N622,N632,N642,C1,C2,C3,C11,C13,C14,C21,C22,C23,C24,C33,
 C34,C41,C42,C43,C44,C52,C62,C63,C100,C101,C102,C211,C221,C231,C241,C421,C423,
 C431,C432,C433,C434,C441,C444,C614,C621,C623,C624,C631,C633,C643,C412,C413,
 C414,C422,C424,C442,C443,C611,C613,C634,C641,C644,B1,B1A)
7.b Ternary CH refined with riding coordinates:
 N622(H622), N632(H632)
7.c Secondary CH2 refined with riding coordinates:
 C614(H61A,H61B), C621(H62A,H62B), C623(H62C,H62D), C624(H62E,H62F), C631(H63A,
 H63B), C633(H63C,H63D), C643(H64A,H64B), C611(H61C,H61D), C613(H61E,H61F),
 C634(H63E,H63F), C641(H64C,H64D), C644(H64E,H64F)
7.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C51(H51), C53(H53), C54(H54), C20A(H20A), C20B(H20B),
 C33(H33), C34(H34), C52(H52), C102(H102), C211(H211), C221(H221), C231(H231),
 C241(H241)
7.e Idealised Me refined as rotating group:
 C200(H20C,H20D,H20E), C201(H20F,H20G,H20H), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C),
 C3(H3A,H3B,H3C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F), C423(H42A,H42B,
 H42C), C432(H43A,H43B,H43C), C433(H43D,H43E,H43F), C434(H43G,H43H,H43I),
 C444(H44A,H44B,H44C), C412(H41A,H41B,H41C), C413(H41D,H41E,H41F), C414(H41G,
 H41H,H41I), C422(H42D,H42E,H42F), C424(H42G,H42H,H42I), C442(H44D,H44E,H44F),
 C443(H44G,H44H,H44I)
7.f Idealised tetrahedral OH refined as rotating group:
 O213(H213), O223(H223), O233(H233), O243(H243)
;
_shelx_res_checksum              54480
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'