F430 Model Chemistry. A Reexamination of the [1,4,7,10,13-Pentaazacyclohexadecane-14,16-dionato(2-)]nickel(II)-Induced Formation of Methane from Methyl Coenzyme-M
Zhong Zhang; Jeffrey L. Petersen; Alan M. Stolzenberg; Inorganic Chemistry 35 (1996) 4649–4655; doi:10.1021/ic960263n

data_4323874
_publ_section_title
;
 F430 Model Chemistry. A Reexamination of the
 [1,4,7,10,13-Pentaazacyclohexadecane-14,16-dionato(2-)]nickel(II)-Induced
 Formation of Methane from Methyl Coenzyme-M
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4649
_journal_page_last               4655
_journal_paper_doi               10.1021/ic960263n
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C15 H29 N5 Ni O6'
_chemical_formula_weight         434.14
_chemical_name_systematic
;
 [1,4,7,10,13-pentaazacyclohexadecane-14,16-dione]nickel(II)diacetate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.234(1)
_cell_length_b                   13.439(2)
_cell_length_c                   18.915(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2083.9(5)
_computing_data_collection       'XSCANS 2.0'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3922
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.970
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0008(3)
_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   1.029
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_obs          0.0374
_refine_ls_shift/esd_max         0.266
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.5012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0939
_refine_ls_wR_factor_obs         0.0834
_reflns_number_observed          2754
_reflns_number_total             3652
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960263n_1.cif
_cod_data_source_block           NiL(OAc)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.5012P] 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^)+(0.0425P)^2^+0.5012P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4323874