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_7036151
_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         'C81 H96 Cu3 N15 O12, F6 P, 2(B F4), H2 O'
_chemical_formula_sum            'C81 H98 B2 Cu3 F14 N15 O13 P'
_chemical_formula_weight         1998.95
_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   mixed
_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                 90.051(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.433(5)
_cell_length_b                   28.692(4)
_cell_length_c                   18.949(3)
_cell_measurement_reflns_used    5769
_cell_measurement_temperature    163
_cell_measurement_theta_max      71.7
_cell_measurement_theta_min      6.6
_cell_volume                     9478(3)
_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      163
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: -0.0560
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: -0.0560
scan:
    Number of images: 72
               Slice: 20.0000 - 200.0000
         Image width: 2.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0560
scan:
    Number of images: 52
               Slice: 48.0000 - 178.0000
         Image width: 2.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0560
scan:
    Number of images: 66
               Slice: 20.0000 - 185.0000
         Image width: 2.5000
            Exp time: 120.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 270.0000
                 XTD: 127.4000
              2theta: -0.0560
;
_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      -0.028717
_diffrn_orient_matrix_UB_12      0.028205
_diffrn_orient_matrix_UB_13      -0.016696
_diffrn_orient_matrix_UB_21      0.044802
_diffrn_orient_matrix_UB_22      0.008621
_diffrn_orient_matrix_UB_23      -0.030885
_diffrn_orient_matrix_UB_31      -0.022827
_diffrn_orient_matrix_UB_32      -0.018562
_diffrn_orient_matrix_UB_33      -0.039714
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            70527
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.076
_diffrn_reflns_theta_max         65.076
_diffrn_reflns_theta_min         6.674
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   FS_Process
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             4124
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.422
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.108
_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     1154
_refine_ls_number_reflns         16003
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1783P)^2^+1.4833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2530
_refine_ls_wR_factor_ref         0.2700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12180
_reflns_number_total             16003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02551f2.cif
_cod_data_source_block           1042538_complex5
_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               7036151
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.722
_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
 B1-F7 = B1-F8 = B1-F9 = B1-F10
 1.37671 with sigma of 0.02
 F7-F8 = F7-F9 = F7-F10 = F8-F9 = F8-F10 = F9-F10
 2.248167 with sigma of 0.02
3. Rigid bond restraints
 O1, O0AA, O3, O4, O5, O6, O213, O223, O233, O243, O253, O263, O2W, F1, F2, F3,
  F4, F5, F6, F7, F8, F9, F10, F11, F12, F13, F14, C11, C11P, C12, C12P, C13,
 C13P, C14, C15, C16, C21, C21P, C22, C22P, C23, C23P, C24, C25, C26, C31, C31P,
  C32, C32P, C33, C33P, C34, C35, C36, C41, C41P, C42, C42P, C43, C43P, C44,
 C45, C46, C51, C51P, C52, C52P, C53, C53P, C54, C55, C56, C61, C62, C63, C64,
 C65, C66, C211, C221, C231, C241, C251, C261, C411, C421, C431, C441, C451,
 C461, C611, C613, C614, C621, C623, C624, C631, C633, C634, C641, C643, C644,
 C651, C653, C654, C661, C663, C664
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B2, F11, F12, F13, F14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B2, F11, F12, F13, F14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1.633*FVAR(2)
5.a Riding coordinates:
 O2W(H2WA), O2W(H2WB)
5.b Free rotating group:
 B2(F11,F12,F13,F14)
5.c Ternary CH refined with riding coordinates:
 N612(H612), N642(H642), N652(H652)
5.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), C651(H65A,H65B), C653(H65C,
 H65D), C654(H65E,H65F), C661(H66A,H66B), C663(H66C,H66D), C664(H66E,H66F)
5.e Me refined with riding coordinates:
 C411(H41A,H41B,H41C), C421(H42A,H42B,H42C), C431(H43A,H43B,H43C), C441(H44A,
 H44B,H44C), C451(H45A,H45B,H45C), C461(H46A,H46B,H46C)
5.f Aromatic/amide H refined with riding coordinates:
 C11P(H11P), C12P(H12P), C13P(H13P), C21P(H21P), C22P(H22P), C23P(H23P),
 C31(H31), C31P(H31P), C32(H32), C32P(H32P), C33(H33), C33P(H33P), C34(H34),
 C35(H35), C36(H36), C41P(H41P), C42P(H42P), C43P(H43P), C51(H51), C51P(H51P),
 C52(H52), C52P(H52P), C53(H53), C53P(H53P), C54(H54), C55(H55), C56(H56),
 C211(H211), C221(H221), C231(H231), C241(H241), C251(H251), C261(H261)
5.g Tetrahedral OH refined with riding coordinates:
 O213(H213), O223(H223), O233(H233), O243(H243), O253(H253), O263(H263)
;
_shelx_res_checksum              93615
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'