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_7052299
_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            'C13 H8 N8 O'
_chemical_formula_weight         292.27
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-05-23T16:49:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3523(13)
_cell_length_b                   13.906(3)
_cell_length_c                   16.582(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0213
_cell_measurement_theta_min      2.8546
_cell_volume                     1464.8(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_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.813
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD 4-circle diffractometer'
_diffrn_measurement_method
;
2 omega-scans with kappa -79 deg (chi -58.3 deg), phi 0, 90 deg
;
_diffrn_orient_matrix_UB_11      0.0023475347
_diffrn_orient_matrix_UB_12      0.0204206072
_diffrn_orient_matrix_UB_13      -0.0392189387
_diffrn_orient_matrix_UB_21      -0.0032549648
_diffrn_orient_matrix_UB_22      -0.046710707
_diffrn_orient_matrix_UB_23      -0.0171219786
_diffrn_orient_matrix_UB_31      -0.1115346406
_diffrn_orient_matrix_UB_32      0.0017737217
_diffrn_orient_matrix_UB_33      -0.0003065426
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5457
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         3.18
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9751
_exptl_absorpt_correction_type   empirical
_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)
Scale3 Pack program including interframe scaling, empirical
absorption correction (Blessing) and detector sensitivity correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
fragment of needle, main axis [100], main faces <021>, <011>, unstable in air
;
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.104
_refine_diff_density_min         -0.102
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.04
_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^)+(0.0223P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                817
_reflns_number_total             1241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605030a.txt
_cod_data_source_block           5-c3h6o
_cod_original_cell_volume        1464.9(5)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7052299