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_7232644
_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         'C14 H20 N4 Ni O2, H O4 S, O2 S0.5, O'
_chemical_formula_sum            'C14 H21 N4 Ni O9 S1.5'
_chemical_formula_weight         496.15
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-21 deposited with the CCDC.    2019-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.803(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7139(16)
_cell_length_b                   11.0715(8)
_cell_length_c                   16.0808(12)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.817
_cell_measurement_theta_min      2.345
_cell_volume                     3797.4(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.095
_diffrn_reflns_theta_max         25.095
_diffrn_reflns_theta_min         2.904
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1033 before and 0.0683 after correction. The Ratio of minimum to maximum transmission is 0.8499. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3386
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0443P)^2^+42.6219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2380
_reflns_number_total             3386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc04058c2.cif
_cod_data_source_block           '[(LH)Ni(H2O)2](HSO4)(SO4)'
_cod_original_formula_sum        'C14 H21 N4 Ni O9 S1.50'
_cod_database_code               7232644
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.940
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.87 with sigma of 0.02
 H2WA-H2WB
 1.38 with sigma of 0.04
 Ni1-H2WA \\sim Ni1-H2WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1A \\sim O3A \\sim O3A \\sim O1A \\sim O1A \\sim O2A \\sim O2A: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: O3A(0.5) O1A(0.5)
5.a Rotating group:
 O1W(H1WA,H1WB)
5.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C7(H7A,H7B), C8(H8A,H8B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C12(H12), C4(H4A), C10(H10), C11(H11)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2A)
;
_shelx_res_checksum              46863
_olex2_submission_special_instructions 'No special instructions were received'