The fixation and reduction of dinitrogen using lanthanides: praseodymium and neodymium meso-octaethylporphyrinogen‒dinitrogen complexes
Campazzi, Elisa; Solari, Euro; Floriani, Carlo; Scopelliti, Rosario; Chemical Communications  (1998) 2603–; doi:10.1039/a807405d

data_7110371
_publ_section_title
;
 The fixation and reduction of dinitrogen using lanthanides: praseodymium
 and neodymium meso-octaethylporphyrinogen--dinitrogen complexes
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2603
_journal_paper_doi               10.1039/a807405d
_journal_year                    1998
_chemical_formula_moiety
'Pr2, 2(C36 H48 N4), N2, 2(C4 H10 Na O2), 2(C12 H30 Na O6)'
_chemical_formula_sum            'C104 H176 N10 Na4 O16 Pr2'
_chemical_formula_weight         2196.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.134(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.1877(14)
_cell_length_b                   19.2513(14)
_cell_length_c                   29.745(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      5.00
_cell_volume                     11530.0(14)
_computing_cell_refinement
'KUMARED, release 1.4.1, 1998, Kuma Diffraction Instruments GMBH'
_computing_data_collection
;
KUMA4CCD, 1998, Kuma Diffraction Instruments GMBH, PSE-EPFL module 3.4,
CH-1015, Lausanne, Switzerland
;
_computing_data_reduction        KUMARED
_computing_molecular_graphics
'XP, Interactive Molecular Graphics, release 5.1, 1998'
_computing_publication_material
'XCIF, SHELXTL release 5.1, 1997, Bruker AXS, Inc.'
_computing_structure_refinement
'SHELXL-97-2 PC version (G. M. Sheldrick, 1998)'
_computing_structure_solution
'SHELXS-97 (G. M. Sheldrick, 1990, Acta Crystallogr., A46, 467)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'KUMA CCD'
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            73129
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.43
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.44
_refine_diff_density_max         '1.962 e\%A^-3^ (0.74\%A from Pr2)'
_refine_diff_density_min         -1.835
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1226
_refine_ls_number_reflns         22661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+94.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                16219
_reflns_number_total             22661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807405dsup1.cif
_cod_data_source_block           total
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        11529.8(14)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110371