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_7001305
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.3350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8224(6)
_cell_length_b                   11.9637(5)
_cell_length_c                   47.332(2)
_cell_measurement_reflns_used    5119
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20.0135
_cell_measurement_theta_min      2.252
_cell_volume                     7820.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1535
_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            73859
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    6.779
_exptl_absorpt_correction_T_max  0.5226
_exptl_absorpt_correction_T_min  0.4101
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         13802
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                6377
_reflns_number_total             13802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900950g.txt
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7001305