Synthesis and Electronic Investigation of Mono- and Di-substituted 4-Nitro- and 4-Amino-bis(pyrazol-1-yl)pyridine-type Ligands and Luminescent Eu(III) Derivatives
Strohecker, Daniel; Lynch, Vincent; Holliday, Bradley; Jones, Richard A.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01153A

data_7043155
_publ_section_title
;
 Synthesis and Electronic Investigation of Mono- and Di-substituted
 4-Nitro- and 4-Amino-bis(pyrazol-1-yl)pyridine-type Ligands and
 Luminescent Eu(III) Derivatives
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01153A
_journal_year                    2017
_chemical_formula_moiety         'C8 H5 Br N4 O2'
_chemical_formula_sum            'C8 H5 Br N4 O2'
_chemical_formula_weight         269.07
_chemical_melting_point          409.9(7)
_chemical_name_common            NO2-pz-py-Br
_chemical_name_systematic        2-bromo-6-(4-pyrazol-1-yl)pyridine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-21 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                77.698(7)
_cell_angle_beta                 81.398(7)
_cell_angle_gamma                75.758(7)
_cell_formula_units_Z            2
_cell_length_a                   5.1820(14)
_cell_length_b                   8.556(3)
_cell_length_c                   11.285(3)
_cell_measurement_reflns_used    6902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.00
_cell_volume                     471.3(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

Sir2004.  Burla M.C., Caliandro, R., Camalli M., Carrozzini, B., Cascarano G.L., 
De Caro, L., Giacovazzo C., Polidori G., Spagna R. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6902
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.367
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'sealed fine focus tube'
_exptl_absorpt_coefficient_mu    4.344
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       bladed
_exptl_crystal_F_000             264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.2750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2010
_reflns_number_total             2125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01153a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '409.25 - 410.65' was changed to
'409.9(7)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7043155
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.282
_shelx_estimated_absorpt_t_max   0.825
_shelx_res_checksum              4283