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_7110372
_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
'Nd2, 2(C36 H48 N4), N2, 2(C8 H16 O4 Na), 2(C4 H8 O2 Na), 7(C4 H8 O2)'
_chemical_formula_sum            'C124 H200 N10 Na4 Nd2 O26'
_chemical_formula_weight         2627.38
_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                 94.02(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.908(3)
_cell_length_b                   15.537(2)
_cell_length_c                   32.885(9)
_cell_measurement_reflns_used    'whole data set'
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      1.24
_cell_volume                     6579(3)
_computing_cell_refinement
;
HKL package, release 1.9.1,
Z. Otwinowski & W. Minor, Methods in Enzymology, Volume 276: Macromolecular
Crystallography, part A,
p. 307-326, 1997, C. W. Jr. Carter & R. M. Sweet, Eds., Academic Press
;
_computing_data_collection
'mar345, 1997, HKL Research Inc., 455 Rockwood Dr. Charlottesville VA 22903'
_computing_data_reduction        'HKL package, release 1.9.1, 1997'
_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  'mar345 area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            49510
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         1.24
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.27
_refine_diff_density_max         '1.207 e\%A^-3^ (0.02\%A from Nd1)'
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.215
_refine_ls_extinction_coef       0.0088(5)
_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   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         10692
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+4.2885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1623
_reflns_number_gt                8471
_reflns_number_total             10692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807405dsup1.cif
_cod_data_source_block           (8)
_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_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110372