Thermodynamic and Kinetic Studies of H2 and N2 Binding to Bimetallic Nickel-Group 13 Complexes and Neutron Structure of a Ni(η2-H2) Adduct
Cammarota, Ryan; Xie, Jing; Burgess, Samantha; Vogiatzis, Konstantinos; Ye, Jingyun; Vollmer, Matthew; Linehan, John C.; Appel, Aaron M.; hoffmann, christina; Wang, Xiaoping; Young, Jr., Victor; Lu, Connie; Chemical Science  (2019) –; doi:10.1039/C9SC02018G

data_1551308
_publ_section_title
;
 Thermodynamic and Kinetic Studies of H2 and N2 Binding to Bimetallic
 Nickel-Group 13 Complexes and Neutron Structure of a Ni(\h2-H2) Adduct
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02018G
_journal_year                    2019
_chemical_formula_moiety         'C39 H62 In N4 Ni P3'
_chemical_formula_sum            'C39 H62 In N4 Ni P3'
_chemical_formula_weight         853.36
_chemical_name_common            H2NiInL
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-01-09 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2010(10)
_cell_length_b                   14.5638(12)
_cell_length_c                   22.547(2)
_cell_measurement_reflns_used    8187
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.68
_cell_measurement_theta_min      7.40
_cell_volume                     4006.4(6)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.658
_diffrn_measured_fraction_theta_max 0.437
_diffrn_measurement_device_type  TOPAZ
_diffrn_measurement_method       'time-of-flight Laue'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.60
_diffrn_radiation_wavelength_details 'Based on neutron time of flight'
_diffrn_reflns_av_R_equivalents  0.1428
_diffrn_reflns_av_unetI/netI     0.3186
_diffrn_reflns_Laue_measured_fraction_full 0.658
_diffrn_reflns_Laue_measured_fraction_max 0.437
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14303
_diffrn_reflns_point_group_measured_fraction_full 0.602
_diffrn_reflns_point_group_measured_fraction_max 0.386
_diffrn_reflns_theta_full        57.140
_diffrn_reflns_theta_max         78.740
_diffrn_reflns_theta_min         7.352
_diffrn_source                   'The ORNL Spallation Neutron Scource'
_exptl_absorpt_coefficient_mu    0.2876
_exptl_absorpt_correction_T_max  0.9343
_exptl_absorpt_correction_T_min  0.8275
_exptl_absorpt_process_details
; 
C. W. Dwiggins, Jr., Acta Cryst. A31, 395 (1975).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.613
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         4718
_refine_ls_number_restraints     1068
_refine_ls_restrained_S_all      0.568
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.607
_reflns_Friedel_fraction_full    0.532
_reflns_Friedel_fraction_max     0.324
_reflns_number_gt                3111
_reflns_number_total             4718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02018g2.cif
_cod_data_source_block           4n
_cod_database_code               1551308
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.988
_exptl_absorpt_special_details
; 
Neutron linear absorption coefficient is wavelength dependent.
For each peak, the absorption coefficient mu is calculated as:
          mu = 1.5700 + 2.3490/1.7982 * wavelength  [cm^-1^]
where 
 1.5700 cm^-1 is the absorption coefficient for total scattering;
 2.3490 cm^-1 is the absorption coefficient for true absorption at 1.7982 A.
 
The value of 0.2876 (mm^-1^) shown in _exptl_absorpt_coefficient_mu 
is the sample absorption coefficient for neutron wavelength at 1.0 \%A.
;
_shelxl_version_number           2014/6
_shelx_res_checksum              26438