Versatility and dynamics of the copper(i) coordination sphere in sterically hindering tris(pyrazolyl)methane-incorporating macrobicycles
Wang, Leyong; Chambron, Jean-Claude; Espinosa, Enrique; New Journal of Chemistry 33 (2009) 327–; doi:10.1039/b816275a

data_7051636
_publ_section_title
;
 Versatility and dynamics of the copper(i) coordination sphere in
 sterically hindering tris(pyrazolyl)methane-incorporating
 macrobicycles
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              327
_journal_paper_doi               10.1039/b816275a
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety
'2(C40 H34 N6 S3),1.5(H2 O),0.5(C2 H6 O),0.5(C H2 Cl2)'
_chemical_formula_sum            'C81.5 H75 Cl N12 O2 S6'
_chemical_formula_weight         1482.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.5750(10)
_cell_angle_beta                 94.080(2)
_cell_angle_gamma                116.7390(10)
_cell_formula_units_Z            2
_cell_length_a                   16.0914(3)
_cell_length_b                   16.2811(4)
_cell_length_c                   16.9439(6)
_cell_measurement_reflns_used    26033
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.65
_cell_volume                     3817.07(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26033
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.542
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         14444
_refine_ls_number_restraints     383
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+6.9158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2127
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                9696
_reflns_number_total             14444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b816275a.txt
_cod_data_source_block           lw077a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3817.06(18)
_cod_original_formula_sum        'C81.50 H75 Cl N12 O2 S6'
_cod_database_code               7051636