Double template effect in [4 + 4] Schiff base macrocycle formation; an ESI-MS study.
Barreira-Fontecha, Julia; Kulmaczewski, Rafal; Ma, Xiaomei; McKee, Vickie; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12040–12043; doi:10.1039/c1dt11341k

data_7017401
_publ_section_title
;
 Double template effect in [4 + 4] Schiff base macrocycle formation; an
 ESI-MS study.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12040
_journal_page_last               12043
_journal_paper_doi               10.1039/c1dt11341k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C115 H163 Ba Cu4 N8 O22'
_chemical_formula_weight         2401.03
_chemical_name_systematic
;

?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.949(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   41.415(9)
_cell_length_b                   42.163(9)
_cell_length_c                   28.256(6)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.15
_cell_measurement_theta_min      3.84
_cell_volume                     48271(18)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.84640
_diffrn_reflns_av_R_equivalents  0.1529
_diffrn_reflns_av_sigmaI/netI    0.1669
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            103961
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.65
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             20112
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Electron count (>10 in voids >100 A^3) = 2364 e/cell
= 296/asymmetric unit or 148/formula unit.
Modelled as 2Et2O, 2OH-, H2O, 2MeOH per formula unit (148e)
Et2O likely in view of the instability of the crystals out of solvent
2OH- needed for charge balance
other H2O/MeOH already observed in non-disordered sites
;
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2395
_refine_ls_number_reflns         25090
_refine_ls_number_restraints     3305
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2658
_refine_ls_wR_factor_ref         0.2936
_reflns_number_gt                10547
_reflns_number_total             25090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11341k.txt
_cod_data_source_block           Complex_2(4msq)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7017401