NewN,N,N-Heteroscorpionates Based on 2,2‘-Bis(pyrazolyl)ethanamine and Its Derivatives. Ligands Designed for Probing Supramolecular Interactions
Reger, Daniel L.; Semeniuc, Radu F.; Gardinier, James R.; O'Neal, Jennifer; Reinecke, Bryn; Smith, Mark D.; Inorganic Chemistry 45 (2006) 4337–4339; doi:10.1021/ic060347o

data_4332417
_publ_section_title
;
 NewN,N,N-Heteroscorpionates Based on 2,2&#x2018;-Bis(pyrazolyl)ethanamine
 and Its Derivatives. Ligands Designed for Probing Supramolecular
 Interactions
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4337
_journal_page_last               4339
_journal_paper_doi               10.1021/ic060347o
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C33 H32 Cu N5 P, N O3, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C34.5 H35 Cl3 Cu N6 O3 P'
_chemical_formula_weight         782.54
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.3510(10)
_cell_angle_beta                 86.1710(10)
_cell_angle_gamma                83.4280(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3448(5)
_cell_length_b                   11.0671(6)
_cell_length_c                   19.4718(11)
_cell_measurement_reflns_used    7074
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.380
_cell_measurement_theta_min      2.624
_cell_volume                     1771.83(17)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19189
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+1.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                6703
_reflns_number_total             7256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060347osup2.cif
_cod_data_source_block           04s024s
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_formula_sum        'C34.50 H35 Cl3 Cu N6 O3 P'
_cod_database_code               4332417