Cooperative Dinitrogen Capture by a Diboraanthracene/Samarocene Pair
Xu, Song; Essex, Laura; Nguyen, Joseph; Farias, Phillip; Ziller, Joseph W.; Harman, Hill; Evans, William J.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03220H

data_7708587
_publ_section_title
;
 Cooperative Dinitrogen Capture by a Diboraanthracene/Samarocene Pair
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03220H
_journal_year                    2021
_chemical_formula_sum            'C68 H104 B2 N2 O2 Sm2'
_chemical_formula_weight         1303.85
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-01-29 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.1061(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.853(2)
_cell_length_b                   21.946(3)
_cell_length_c                   17.947(2)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.22
_cell_volume                     6514.8(14)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 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 SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39023
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.831
_diffrn_reflns_theta_min         1.542
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
'layering hexane over toluene solution'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.164
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         8043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+6.4041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6387
_reflns_number_total             8043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03220h2.cif
_cod_data_source_block           sx3
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        6514.7(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7708587
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.661
_shelx_estimated_absorpt_t_max   0.754
_exptl_absorpt_special_details
; 
Reflections not merged 
39584 Corrected reflections written to file sx3s.hkl 
Estimated minimum and maximum transmission:  0.6593  0.7458 
The ratio (0.8840) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              85757