A Stable Monomeric Nickel Borohydride
Patrick J. Desrochers; Stacey LeLievre; Rosemary J. Johnson; Brian T. Lamb; Andrea L. Phelps; A. W. Cordes; Weiwei Gu; Stephen P. Cramer; Inorganic Chemistry 42 (2003) 7945–7950; doi:10.1021/ic034687a

data_4312607
_publ_section_title
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 A Stable Monomeric Nickel Borohydride
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7945
_journal_page_last               7950
_journal_paper_doi               10.1021/ic034687a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         Tp*NiCl
_chemical_formula_sum            'C15 H22 B Cl N6 Ni'
_chemical_formula_weight         391.36
_chemical_name_systematic
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 ? 
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_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P -2a 2a'
_symmetry_space_group_name_H-M   'P 21 m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4467(4)
_cell_length_b                   13.1553(2)
_cell_length_c                   8.0191(7)
_cell_measurement_reflns_used    12975
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1840.52(17)
_computing_cell_refinement       'CrystalClear (Rigaku Corp, 1999)'
_computing_data_collection       'CrystalClear (Rigaku Corp, 1999)'
_computing_data_reduction        'Texsan (Molecular Structure Corp, 1998)'
_computing_molecular_graphics    'Ortep3,v1.05, L.J.Farrugia,UnivGlasgow'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'Mercury CCD - AFC8S'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2548
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   'empirical, R.A.Jacobson, MS Corp, 1998'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                2093
_reflns_number_total             2547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034687asi20030617_043843_2.cif
_cod_data_source_block           Tp*NiCl
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0445P)^2^] where P=(Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4312607