Metal String Complexes: Synthesis and Crystal Structure of [Ni4(μ4-phdpda)4] and [Ni7(μ7-teptra)4Cl2] (H2phdpda = N-Phenyldipyridyldiamine and H3teptra = Tetrapyridyltriamine)
Shie-Yang Lai; Tzu-Wei Lin; Yu-Hua Chen; Chih-Chieh Wang; Gene-Hsiang Lee; Ming-hwa Yang; Man-kit Leung; Shie-Ming Peng; Journal of the American Chemical Society 121 (1999) 250–251; doi:10.1021/ja982065w

data_4116277
_publ_section_title
;
 Metal String Complexes: Synthesis and Crystal Structure of
 [Ni4(\m4-phdpda)4] and [Ni7(\m7-teptra)4Cl2] (H2phdpda =
 N-Phenyldipyridyldiamine and H3teptra = Tetrapyridyltriamine)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              250
_journal_page_last               251
_journal_paper_doi               10.1021/ja982065w
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C83 H59 Cl11 N28 Ni7'
_chemical_formula_weight         2249.50
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.8680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.7542(7)
_cell_length_b                   16.9432(5)
_cell_length_c                   28.5946(9)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     9520.4(5)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38984
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        3
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.215
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         16710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.215
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_obs          0.0824
_refine_ls_shift/esd_max         0.098
_refine_ls_shift/esd_mean        0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1663P)^2^+12.7629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3020
_refine_ls_wR_factor_obs         0.2460
_reflns_number_observed          8931
_reflns_number_total             16710
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982065w_2.cif
_cod_data_source_block           ic5585
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1663P)^2^+12.7629P] 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^)+(0.1663P)^2^+12.7629P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116277