Dinitrogen Reduction, Sulfur Reduction, and Isoprene Polymerization via Photochemical Activation of Trivalent Bis(cyclopentadienyl) Rare-Earth-Metal Allyl Complexes
Fieser, Megan E.; Johnson, Casey W.; Bates, Jefferson E.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Organometallics 34 (2015) 4387–; doi:10.1021/acs.organomet.5b00613

data_4087817
_publ_section_title
;
 Dinitrogen Reduction, Sulfur Reduction, and Isoprene Polymerization via
 Photochemical Activation of Trivalent Bis(cyclopentadienyl)
 Rare-Earth-Metal Allyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4387
_journal_paper_doi               10.1021/acs.organomet.5b00613
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C40 H60 Lu2 S'
_chemical_formula_weight         922.88
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6701(7)
_cell_length_b                   14.6701(7)
_cell_length_c                   18.9233(9)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      29.02
_cell_measurement_theta_min      2.56
_cell_volume                     4072.5(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.9-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXT 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49601
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.200
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.894
_exptl_absorpt_correction_T_max  0.6345
_exptl_absorpt_correction_T_min  0.3881
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/4'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
; 
 Flack x determined using 2280 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+0.6026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0334
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                5208
_reflns_number_total             5330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00613_si_003.cif
_cod_data_source_block           mef29
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4072.5(4)
_cod_database_code               4087817
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.246
_shelx_estimated_absorpt_t_max   0.582
_shelx_res_checksum              28189
_shelx_hkl_checksum              95830
_shelx_fab_checksum              49825