Synthesis, Structure, and15N NMR Studies of Paramagnetic Lanthanide Complexes Obtained by Reduction of Dinitrogen
Evans, William J.; Rego, Daniel B.; Ziller, Joseph W.; Inorganic Chemistry 45 (2006) 10790–10798; doi:10.1021/ic061485g

data_4333139
_publ_section_title
;
 Synthesis, Structure, and15N NMR Studies of Paramagnetic Lanthanide
 Complexes Obtained by Reduction of Dinitrogen
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10790
_journal_page_last               10798
_journal_paper_doi               10.1021/ic061485g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C58 H84 N2 O2 Pr2'
_chemical_formula_weight         1123.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
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_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90.00
_cell_angle_beta                 104.177(2)
_cell_angle_gamma                90.00
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_cell_length_a                   15.3137(18)
_cell_length_b                   14.1046(17)
_cell_length_c                   12.8773(15)
_cell_measurement_temperature    163(2)
_cell_volume                     2696.7(6)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0232
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_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
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_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multi-faceted-polyhedra
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.35
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_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.197
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         6197
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_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+24.9754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                5802
_reflns_number_total             6197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061485gsup6.cif
_cod_data_source_block           dbr32
_cod_depositor_comments
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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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4333139