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_7232641
_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         'C18 H22 N6 Ni, 2(C24 H20 B), C2 H3 N'
_chemical_formula_sum            'C68 H65 B2 N7 Ni'
_chemical_formula_weight         1060.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-09 deposited with the CCDC.    2019-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                98.7500(10)
_cell_angle_beta                 101.4640(10)
_cell_angle_gamma                103.6170(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5825(5)
_cell_length_b                   13.5215(6)
_cell_length_c                   19.6576(8)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.30
_cell_volume                     2867.7(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker 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  0.0398
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35330
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.090
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1176 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.8516. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         10208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0419
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8203
_reflns_number_total             10208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc04058c2.cif
_cod_data_source_block           '[(LH)Ni(CH3CN)2](BPh4)2'
_cod_database_code               7232641
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N4(H4), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00R(H00C,H00D), C00U(H00F,H00G), C01Q(H01A,H01B)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00C(H00H), C00E(H00E), C00G(H00J), C00I(H00I), C00J(H00K),
 C00M(H00M), C00N(H00N), C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T),
 C00V(H00V), C00W(H00W), C00Z(H00Z), C010(H010), C012(H012), C014(H014),
 C015(H015), C017(H017), C018(H018), C019(H019), C01A(H01J), C01B(H01G),
 C01C(H01C), C01D(H01M), C01E(H01H), C01F(H01P), C01G(H01I), C01H(H01Q),
 C01I(H01S), C01J(H01T), C01K(H01K), C01L(H01L), C01M(H01U), C01N(H01N),
 C01O(H01O), C01P(H01W), C01R(H01R), C01S(H01Z), C01T(H01), C01U(H0AA),
 C01V(H01V), C01X(H01X), C01Y(H01Y), C021(H021)
2.d Idealised Me refined as rotating group:
 C01Z(H01D,H01E,H01F), C020(H02D,H02E,H02F), C025(H02A,H02B,H02C)
;
_shelx_res_checksum              35452
_olex2_submission_special_instructions 'No special instructions were received'