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_7036150
_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 Br Cu2 N8 O8, 1.17(C2 H6 O S), 0.83(H2 O), Br, C H4 O'
_chemical_formula_sum            'C59.33 H90.67 Br2 Cu2 N8 O11 S1.17'
_chemical_formula_weight         1416.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-03
_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                 97.390(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4887(3)
_cell_length_b                   28.5296(5)
_cell_length_c                   17.2548(12)
_cell_measurement_reflns_used    27230
_cell_measurement_temperature    123
_cell_measurement_theta_max      72.0
_cell_measurement_theta_min      6.5
_cell_volume                     7561.3(6)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
scan:
    Number of images: 55
               Slice: 20.0000 - 185.0000
         Image width: 3.0000
            Exp time: 96.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 50
               Slice: 20.0000 - 170.0000
         Image width: 3.0000
            Exp time: 96.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 60
               Slice: 20.0000 - 200.0000
         Image width: 3.0000
            Exp time: 96.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 56
               Slice: 24.0000 - 194.0000
         Image width: 3.0000
            Exp time: 96.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 49
               Slice: 21.0000 - 168.0000
         Image width: 3.0000
            Exp time: 96.0000
       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      0.036818
_diffrn_orient_matrix_UB_12      -0.004105
_diffrn_orient_matrix_UB_13      0.051564
_diffrn_orient_matrix_UB_21      0.002388
_diffrn_orient_matrix_UB_22      0.034787
_diffrn_orient_matrix_UB_23      0.007054
_diffrn_orient_matrix_UB_31      -0.053640
_diffrn_orient_matrix_UB_32      -0.001269
_diffrn_orient_matrix_UB_33      0.026583
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_laue_measured_fraction_full 0.986
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            83050
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        58.930
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_min         6.546
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           20.0
_diffrn_source_power             0.8
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   FS_Process
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       Block
_exptl_crystal_F_000             2949
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         10698
_refine_ls_number_restraints     610
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1502P)^2^+21.0226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7522
_reflns_number_total             10698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02551f2.cif
_cod_data_source_block           1042537_Complex2
_cod_depositor_comments
'Adding full bibliography for 7036149--7036153.cif.'
_cod_database_code               7036150
_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, All O(H,H) groups
2. Restrained distances
 C441-C442 = C441-C443 = C441-C444
 1.49091 with sigma of 0.02
 C442-C443 = C442-C444 = C443-C444
 2.434656 with sigma of 0.02
 C445-C446 = C445-C447 = C446-C447
 2.434656 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, C221, C231, C241, C411,
 C412, C413, C414, C421, C422, C423, C424, C431, C432, C433, C434, C441, C4, C5,
  C443, C444, C442, C446, C445, C447, C1, C611, C613, C614, C621, C623, C624,
 C631, C633, C634, C641, C643, C644, C2M, C2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C414 \\sim C413 \\sim C412: within 1.2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O644: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.005
C2M \\sim O1M: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004
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(C221) \\sim Ueq, Uanis(C231) \\sim Ueq, Uanis(C241) \\sim Ueq,
Uanis(C411) \\sim Ueq, Uanis(C412) \\sim Ueq, Uanis(C413) \\sim Ueq,
Uanis(C414) \\sim Ueq, Uanis(C421) \\sim Ueq, Uanis(C422) \\sim Ueq,
Uanis(C423) \\sim Ueq, Uanis(C424) \\sim Ueq, Uanis(C431) \\sim Ueq,
Uanis(C432) \\sim Ueq, Uanis(C433) \\sim Ueq, Uanis(C434) \\sim Ueq,
Uanis(C441) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C443)
\\sim Ueq, Uanis(C444) \\sim Ueq, Uanis(C442) \\sim Ueq, Uanis(C446) \\sim Ueq,
Uanis(C445) \\sim Ueq, Uanis(C447) \\sim Ueq, Uanis(C1) \\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(C2M) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O213) \\sim Ueq, Uanis(O223) \\sim Ueq, Uanis(O233)
\\sim Ueq, Uanis(O243) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1W) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(O1M) \\sim Ueq, Uanis(O644) \\sim Ueq: with sigma of
0.0075 and sigma for terminal atoms of 0.015
Uanis(O644) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Sof(C446)=Sof(H44J)=Sof(H44K)=Sof(H44L)=Sof(C445)=Sof(H44M)=Sof(H44N)=
 Sof(H44O)=Sof(C447)=Sof(H44P)=Sof(H44Q)=Sof(H44R)=1-FVAR(2)
 Sof(C443)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C444)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C442)=Sof(H44G)=Sof(H44H)=Sof(H44I)=FVAR(2)
 Fixed Sof: S0AA(0.5) O3(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) H5C(0.5) O1W(0.5) H1WA(0.5) H1WB(0.5) S1(0.6667) O1(0.6667)
 C1(0.6667) H1A(0.6667) H1B(0.6667) H1C(0.6667) O644(0.33333) H64G(0.33333)
 H64H(0.33333) C2(0.6667) H2A(0.6667) H2B(0.6667) H2C(0.6667)
6.a Riding coordinates:
 O233(H233), O243(H243), O1W(H1WA), O1W(H1WB), O1M(H1M), O644(H64G),
 O644(H64H), C2(H2A), C2(H2B), C2(H2C)
6.b Free rotating group:
 S0AA(O3,C4,C5,C443,C444,C442,C446,C445,C447,O1W), S1(O1,C1,C611,C613,C614,
 C621,C623,C624,C631,C633,C634,C641,C643,C644,Br2)
6.c Ternary CH refined with riding coordinates:
 N622(H622), N632(H632)
6.d 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.e Me refined with riding coordinates:
 C443(H44A,H44B,H44C), C444(H44D,H44E,H44F), C442(H44G,H44H,H44I), C446(H44J,
 H44K,H44L), C445(H44M,H44N,H44O), C447(H44P,H44Q,H44R)
6.f 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), C221(H221), C231(H231), C241(H241)
6.g Idealised Me refined as rotating group:
 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), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C1(H1A,H1B,H1C), C2M(H2MA,H2MB,H2MC)
6.h Idealised tetrahedral OH refined as rotating group:
 O213(H213), O223(H223)
;
_shelx_res_checksum              28364
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'