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_7232647
_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_absolute_configuration unk
_chemical_formula_moiety         '3(C29 H27 N4 Ni O2), C4 H10 O, 3(C24 H20 B)'
_chemical_formula_sum            'C163 H151 B3 N12 Ni3 O7'
_chemical_formula_weight         2598.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-20
_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                90
_cell_angle_beta                 93.976(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   42.319(3)
_cell_length_b                   22.6000(14)
_cell_length_c                   15.7228(9)
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.643
_cell_measurement_theta_min      2.385
_cell_volume                     15001.2(17)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            90580
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.757
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1579 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.9095. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.125
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.551(13)
_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     1686
_refine_ls_number_reflns         26417
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+28.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                22890
_reflns_number_total             26417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc04058c2.cif
_cod_data_source_block           '[(LH)Ni(dbm)](BPh4)'
_cod_original_cell_volume        15001.4(17)
_cod_database_code               7232647
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.449(13)
 0.551(13)
2. 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
3. Uiso/Uaniso restraints and constraints
C38 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
O7 \\sim C89 \\sim C90 \\sim C91 \\sim C92: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
O1B \\sim C64 \\sim C65 \\sim C63 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim
C62: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Ni1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.05
4.a Ternary CH refined with riding coordinates:
 N2A(H2A), N4A(H4A), N4(H4), N2(H2), N2C(H2C), N2B(H2B)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C57(H57A,H57B), C44(H44A,H44B), C7(H7A,H7B),
 C8(H8A,H8B), C0AA(H0AA,H0AB), C1(H1A,H1B), C82(H82A,H82B), C81(H81A,H81B),
 C66(H66A,H66B), C72(H72A,H72B), C89(H89A,H89B), C91(H91A,H91B)
4.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C43(H43),
 C42(H42), C41(H41), C40(H40), C39(H39), C46(H46), C47(H47), C48(H48), C55(H55),
  C54(H54), C53(H53), C21(H21), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C3(H3), C4(H4B),
 C5(H5), C12(H12), C11(H11), C10(H10), C80(H80), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C2BA(H2BA), C84(H84), C4BA(H4BA), C65(H65), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C68(H68), C69(H69), C70(H70), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C100(H100), C101(H101), C102(H102),
 C103(H103), C104(H104), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116),
 C118(H118), C119(H119), C120(H120), C121(H121), C122(H122), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C130(H130), C131(H131),
 C132(H132), C133(H133), C134(H134), C136(H136), C137(H137), C138(H138),
 C139(H139), C140(H140), C142(H142), C143(H143), C144(H144), C145(H145),
 C146(H146), C148(H148), C149(H149), C150(H150), C151(H151), C152(H152),
 C154(H154), C155(H155), C156(H156), C157(H157), C158(H158), C160(H160),
 C161(H161), C162(H162), C163(H163), C164(H164)
4.d Fitted hexagon refined as free rotating group:
 C63(C58,C59,C60,C61,C62)
4.e Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              41226
_shelx_fab_checksum              81296
_olex2_submission_special_instructions 'No special instructions were received'