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_4341461
_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            'C11 H11 Cl N5 O7 Re'
_chemical_formula_weight         546.90
_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                90.653(6)
_cell_angle_beta                 93.547(6)
_cell_angle_gamma                109.830(8)
_cell_formula_units_Z            2
_cell_length_a                   8.0258(6)
_cell_length_b                   10.7509(9)
_cell_length_c                   10.7993(7)
_cell_measurement_reflns_used    1857
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.7112
_cell_measurement_theta_min      4.1005
_cell_volume                     874.36(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5044
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         74.89
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.424
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.2343
_exptl_crystal_size_mid          0.1630
_exptl_crystal_size_min          0.0679
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                2849
_reflns_number_total             3398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5018054_si_003.cif
_cod_data_source_block           4a
_cod_original_cell_volume        874.36(11)
_cod_database_code               4341461