Syntheses, structural characterisation and magnetic properties of Fe(<small>II</small>) and Mn(<small>II</small>) compounds with the pentacyanopropenido ligand; structural characterisation of a substituted pyrazolo[1,5-<i>a</i>]pyrimidine
Emeric Lefebvre; Françoise Conan; Nathalie Cosquer; Jean-Michel Kerbaol; Mathieu Marchivie; Jean Sala-Pala; Marek M. Kubicki; Estelle Vigier; Carlos J. Gomez Garcia; New Journal of Chemistry 30 (2006) 1197–; doi:10.1039/b605030a

data_7052298
_publ_section_title
;
 Syntheses, structural characterisation and magnetic properties of
 Fe(<small>II</small>) and Mn(<small>II</small>) compounds with the
 pentacyanopropenido ligand; structural characterisation of a
 substituted pyrazolo[1,5-<i>a</i>]pyrimidine
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1197
_journal_paper_doi               10.1039/b605030a
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C10 H2 N8'
_chemical_formula_weight         234.2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-05-24T15:11:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.48(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8515(19)
_cell_length_b                   6.5515(18)
_cell_length_c                   19.107(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0512
_cell_measurement_theta_min      2.9712
_cell_volume                     1100.9(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'X-CALIBUR 2 4-circle CCD diffractometer'
_diffrn_measurement_method
;
4 omega-scans with kappa = -79%, phi = 0, 90, 180, 270%
;
_diffrn_orient_matrix_UB_11      0.0468174366
_diffrn_orient_matrix_UB_12      0.0030096129
_diffrn_orient_matrix_UB_13      -0.0278012786
_diffrn_orient_matrix_UB_21      -0.0523527653
_diffrn_orient_matrix_UB_22      -0.0637686862
_diffrn_orient_matrix_UB_23      -0.0206110602
_diffrn_orient_matrix_UB_31      -0.0397266398
_diffrn_orient_matrix_UB_32      0.0873151788
_diffrn_orient_matrix_UB_33      -0.014091838
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6054
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.75
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.99676
_exptl_absorpt_correction_T_min  0.94725
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.13 beta (release 14.11.2003 CrysAlis171 VC++)
(compiled Nov 14 2003,14:35:41)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
rectangular plate, main faces <001>, long edges <100>
;
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.1764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                1230
_reflns_number_total             1577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605030a.txt
_cod_data_source_block           el93e
_cod_original_cell_volume        1101.0(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7052298