A Dinuclear Ni(I) System Having a Diradical Ni2N2 Diamond Core Resting State: Synthetic, Structural, Spectroscopic Elucidation, and Reductive Bond Splitting Reactions
Debashis Adhikari; Susanne Mossin; Falguni Basuli; Benjamin R. Dible; Mircea Chipara; Hongjun Fan; John C. Huffman; Karsten Meyer; Daniel J. Mindiola; Inorganic Chemistry 47 (2008) 10479–10490; doi:10.1021/ic801137p

data_4306290
_publ_section_title
;
A Dinuclear Ni(I) System Having a Diradical Ni2N2 Diamond Core Resting
State: Synthetic, Structural, Spectroscopic Elucidation, and Reductive Bond
Splitting Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10479
_journal_page_last               10490
_journal_paper_doi               10.1021/ic801137p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C43 H60 N3 Ni O P2'
_chemical_formula_weight         755.59
_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                 107.780(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.683(6)
_cell_length_b                   9.239(2)
_cell_length_c                   26.581(8)
_cell_measurement_reflns_used    737
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.35
_cell_volume                     4135(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'   0.30 degree frames measured for 60.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.4633
_diffrn_reflns_av_sigmaI/netI    0.9713
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21448
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.681
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         9498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.681
_refine_ls_R_factor_all          0.3655
_refine_ls_R_factor_gt           0.0926
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                1769
_reflns_number_total             9498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801137p_si_002.cif
_cod_data_source_block           05247
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4306290