Pyrazolylamidino Ligands from Coupling of Acetonitrile and Pyrazoles: A Systematic Study.
Gómez-Iglesias, Patricia; Arroyo, Marta; Bajo, Sonia; Strohmann, Carsten; Miguel, Daniel; Villafañe, Fernando; Inorganic chemistry  (2014) 141107133009008–; doi:10.1021/ic5018054

data_4341463
_publ_section_title
;
 Pyrazolylamidino Ligands from Coupling of Acetonitrile and Pyrazoles: A
 Systematic Study.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141107133009008
_journal_paper_doi               10.1021/ic5018054
_journal_year                    2014
_chemical_formula_sum            'C14.5 H16.5 Cl1.5 F3 N4 O6 Re S'
_chemical_formula_weight         671.26
_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                80.620(5)
_cell_angle_beta                 89.784(5)
_cell_angle_gamma                68.130(6)
_cell_formula_units_Z            4
_cell_length_a                   10.6571(6)
_cell_length_b                   13.8282(8)
_cell_length_c                   17.0627(12)
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8834
_cell_measurement_theta_min      2.0590
_cell_volume                     2297.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.650
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w 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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8093
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.77
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.615
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.5329
_exptl_crystal_size_mid          0.3591
_exptl_crystal_size_min          0.2997
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                5527
_reflns_number_total             7047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5018054_si_003.cif
_cod_data_source_block           5b-OTf
_cod_original_cell_volume        2297.9(2)
_cod_original_formula_sum        'C7.25 H8.25 Cl0.75 F1.50 N2 O3 Re0.50 S0.50'
_cod_database_code               4341463