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_7036153
_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         '4(Br), C80 H95 Cu2 N8 O4, 2(C H4 O)'
_chemical_formula_sum            'C82 H103 Br4 Cu2 N8 O6'
_chemical_formula_weight         1743.44
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-07
_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                 93.644(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1144(4)
_cell_length_b                   24.4307(4)
_cell_length_c                   19.1882(14)
_cell_measurement_reflns_used    42887
_cell_measurement_temperature    140
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      6.6
_cell_volume                     8942.4(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      140
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 68
               Slice: 22.0000 - 192.0000
         Image width: 2.5000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 48
               Slice: 20.0000 - 140.0000
         Image width: 2.5000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 70
               Slice: 22.0000 - 197.0000
         Image width: 2.5000
            Exp time: 90.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 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      0.013569
_diffrn_orient_matrix_UB_12      -0.031403
_diffrn_orient_matrix_UB_13      -0.029726
_diffrn_orient_matrix_UB_21      0.023719
_diffrn_orient_matrix_UB_22      0.025914
_diffrn_orient_matrix_UB_23      -0.031231
_diffrn_orient_matrix_UB_31      0.044737
_diffrn_orient_matrix_UB_32      -0.004215
_diffrn_orient_matrix_UB_33      0.029463
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98204
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        65.081
_diffrn_reflns_theta_max         65.081
_diffrn_reflns_theta_min         6.593
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   FS_Process
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       Block
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.149
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         15072
_refine_ls_number_restraints     1237
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1247P)^2^+12.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12262
_reflns_number_total             15072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02551f2.cif
_cod_data_source_block           1042540_Complex4
_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_database_code               7036153
_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
 C411-C412 = C411-C413 = C411-C414
 1.53395 with sigma of 0.02
 C412-C413 = C412-C414 = C413-C414
 2.50494 with sigma of 0.02
 C421-C422 = C421-C423 = C421-C424
 1.53395 with sigma of 0.02
 C421-C4A = C421-C5A = C421-C6A
 1.53395 with sigma of 0.02
 C422-C423 = C422-C424 = C423-C424
 2.50494 with sigma of 0.02
 C4A-C5A = C4A-C6A = C5A-C6A
 2.50494 with sigma of 0.02
3. Rigid bond restraints
 C11, C12, C13, C14, C21, C22, C23, C24, C31, C32, C33, C34, C41, C42, C43,
 C44, C51, C52, C53, C54, C61, C62, C63, C64, C211, C213, C214, C215, C216,
 C217, C218, C221, C223, C224, C225, C226, C227, C228, C231, C233, C234, C235,
 C236, C237, C238, C241, C243, C244, C245, C246, C247, C248, C411, C421, C431,
 C432, C433, C434, C441, C442, C443, C611, C613, C614, C621, C623, C624, C631,
 C633, C634, C641, C643, C644, C444, C100, C200, C414, C412, C413, C422, C423,
 C424, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
 C11, C12, C13, C14, C21, C22, C23, C24, C31, C32, C33, C34, C41, C42, C43,
 C44, C51, C52, C53, C54, C61, C62, C63, C64, C211, C213, C214, C215, C216,
 C217, C218, C221, C223, C224, C225, C226, C227, C228, C231, C233, C234, C235,
 C236, C237, C238, C241, C243, C244, C245, C246, C247, C248, C411, C421, C431,
 C432, C433, C434, C441, C442, C443, C611, C613, C614, C621, C623, C624, C631,
 C633, C634, C641, C643, C644, C444, C100, C200, C414, C412, C413, C422, C423,
 C424, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C211 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217 \\sim C218 \\sim
C221 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228 \\sim
C231 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C237 \\sim C238 \\sim
C241 \\sim C243 \\sim C244 \\sim C245 \\sim C246 \\sim C247 \\sim C248 \\sim
C411 \\sim C421 \\sim C431 \\sim C432 \\sim C433 \\sim C434 \\sim C441 \\sim
C442 \\sim C443 \\sim C611 \\sim C613 \\sim C614 \\sim C621 \\sim C623 \\sim
C624 \\sim C631 \\sim C633 \\sim C634 \\sim C641 \\sim C643 \\sim C644 \\sim
C444 \\sim C100 \\sim C200 \\sim C414 \\sim C412 \\sim C413 \\sim C422 \\sim
C423 \\sim C424 \\sim C4A \\sim C5A \\sim C6A: within 1.5A with sigma of 0.05
and sigma for terminal atoms of 0.1
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C211 \\sim C213 \\sim C214 \\sim C215 \\sim C216 \\sim C217 \\sim C218 \\sim
C221 \\sim C223 \\sim C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228 \\sim
C231 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C237 \\sim C238 \\sim
C241 \\sim C243 \\sim C244 \\sim C245 \\sim C246 \\sim C247 \\sim C248 \\sim
C411 \\sim C421 \\sim C431 \\sim C432 \\sim C433 \\sim C434 \\sim C441 \\sim
C442 \\sim C443 \\sim C611 \\sim C613 \\sim C614 \\sim C621 \\sim C623 \\sim
C624 \\sim C631 \\sim C633 \\sim C634 \\sim C641 \\sim C643 \\sim C644 \\sim
C444 \\sim C100 \\sim C200 \\sim C414 \\sim C412 \\sim C413 \\sim C422 \\sim
C423 \\sim C424 \\sim C4A \\sim C5A \\sim C6A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 1.7
Uanis(C11) \\sim Ueq, Uanis(C12) \\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(C31) \\sim Ueq, Uanis(C32) \\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(C51) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C61) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C211)
\\sim Ueq, Uanis(C213) \\sim Ueq, Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq,
Uanis(C216) \\sim Ueq, Uanis(C217) \\sim Ueq, Uanis(C218) \\sim Ueq,
Uanis(C221) \\sim Ueq, Uanis(C223) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C225) \\sim Ueq, Uanis(C226) \\sim Ueq, Uanis(C227) \\sim Ueq,
Uanis(C228) \\sim Ueq, Uanis(C231) \\sim Ueq, Uanis(C233) \\sim Ueq,
Uanis(C234) \\sim Ueq, Uanis(C235) \\sim Ueq, Uanis(C236) \\sim Ueq,
Uanis(C237) \\sim Ueq, Uanis(C238) \\sim Ueq, Uanis(C241) \\sim Ueq,
Uanis(C243) \\sim Ueq, Uanis(C244) \\sim Ueq, Uanis(C245) \\sim Ueq,
Uanis(C246) \\sim Ueq, Uanis(C247) \\sim Ueq, Uanis(C248) \\sim Ueq,
Uanis(C411) \\sim Ueq, Uanis(C421) \\sim Ueq, Uanis(C431) \\sim Ueq,
Uanis(C432) \\sim Ueq, Uanis(C433) \\sim Ueq, Uanis(C434) \\sim Ueq,
Uanis(C441) \\sim Ueq, Uanis(C442) \\sim Ueq, Uanis(C443) \\sim Ueq,
Uanis(C611) \\sim Ueq, Uanis(C613) \\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(C634) \\sim Ueq,
Uanis(C641) \\sim Ueq, Uanis(C643) \\sim Ueq, Uanis(C644) \\sim Ueq,
Uanis(C444) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C200) \\sim Ueq,
Uanis(C414) \\sim Ueq, Uanis(C412) \\sim Ueq, Uanis(C413) \\sim Ueq,
Uanis(C422) \\sim Ueq, Uanis(C423) \\sim Ueq, Uanis(C424) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(Br1) \\sim Ueq,
Uanis(Br2) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Br5)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Br5)=1-FVAR(1)
 Sof(Br4)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(2)
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(3)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=1-FVAR(3)
 Sof(C422)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C423)=Sof(H42D)=Sof(H42E)=
 Sof(H42F)=Sof(C424)=Sof(H42G)=Sof(H42H)=Sof(H42I)=FVAR(3)
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 everything fixed:
 C422(H42A,H42B,H42C), C423(H42D,H42E,H42F), C424(H42G,H42H,H42I), C4A(H4AA,
 H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC)
6.d Me refined with riding coordinates:
 C432(H43A,H43B,H43C), C433(H43D,H43E,H43F), C434(H43G,H43H,H43I), C442(H44A,
 H44B,H44C), C443(H44D,H44E,H44F), C444(H44G,H44H,H44I)
6.e Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), 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)
6.f Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C200(H20A,H20B,H20C), C414(H41A,H41B,H41C), C412(H41D,
 H41E,H41F), C413(H41G,H41H,H41I)
6.g Idealised tetrahedral OH refined as rotating group:
 O100(H100), O200(H200)
;
_shelx_res_checksum              37295
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'