Solvent-Free Synthesis and Reactivity of Nickel(II) Borohydride and Nickel(II) Hydride
Angamuthu, Raja; Raje, Sakthi; Green Chemistry  (2019) –; doi:10.1039/C8GC04058C

data_7232640
_publ_section_title
;
 Solvent-Free Synthesis and Reactivity of Nickel(II) Borohydride and
 Nickel(II) Hydride
;
_journal_name_full               'Green Chemistry'
_journal_paper_doi               10.1039/C8GC04058C
_journal_year                    2019
_chemical_formula_moiety         'C28 H32 Ni2 I2 N8, 2(C H4 O), 2(I)'
_chemical_formula_sum            'C30 H40 I4 N8 Ni2 O2'
_chemical_formula_weight         1169.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.098(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.061(4)
_cell_length_b                   10.993(2)
_cell_length_c                   19.320(4)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.352
_cell_measurement_theta_min      2.306
_cell_volume                     3750.9(13)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXT'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Apex 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9432
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.518
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    4.335
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         6.718
_refine_diff_density_min         -7.661
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.459
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         9432
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.457
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.1157
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3284
_refine_ls_wR_factor_ref         0.3700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6860
_reflns_number_total             9432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc04058c2.cif
_cod_data_source_block           '[(LH)Ni(mu-I)2Ni(LH)]I2'
_cod_original_cell_volume        3750.8(12)
_cod_database_code               7232640
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              78952