The problems of detecting hydrides in metal carbonyl clusters by 1H NMR: the case study of [H4−nNi22(C2)4(CO)28(CdBr)2]n− (n = 2‒4)
Bernardi, Alessandro; Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Dalton Transactions  (2009) 4245–4251; doi:10.1039/b900950g

data_7001306
_publ_section_title
;
 The problems of detecting hydrides in metal carbonyl clusters by 1H
 NMR: the case study of [H4&#x2212;nNi22(C2)4(CO)28(CdBr)2]n&#x2212; (n
 = 2--4)
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              4245
_journal_page_last               4251
_journal_paper_doi               10.1039/b900950g
_journal_year                    2009
_chemical_formula_sum            'C52 H40 Br2 Cd2 N2 Ni22 O30'
_chemical_formula_weight         2849.10
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.2840(10)
_cell_angle_beta                 88.1690(10)
_cell_angle_gamma                74.1690(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9025(6)
_cell_length_b                   16.6447(8)
_cell_length_c                   21.3768(10)
_cell_measurement_reflns_used    7255
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.0215
_cell_measurement_theta_min      2.2285
_cell_volume                     3988.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45012
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    6.646
_exptl_absorpt_correction_T_max  0.5027
_exptl_absorpt_correction_T_min  0.3226
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         17303
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                9657
_reflns_number_total             17303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900950g.txt
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001306