[Ni(Et~2~PCH~2~NMeCH~2~PEt~2~)~2~]^2+^ as a Functional Model for Hydrogenases
Calvin J. Curtis; Alex Miedaner; Rebecca Ciancanelli; William W. Ellis; Bruce C. Noll; M. Rakowski DuBois; Daniel L. DuBois; Inorganic Chemistry 42 (2003) 216–227; doi:10.1021/ic020610v

data_4312868
_publ_contact_author_address
;
National Renewable Energy Laboratory
1617 Cole Boulevard
Golden, CO 80401-3393
USA
;
_publ_contact_author_email       Dan_Dubois@nrel.gov
_publ_contact_author_name        'Daniel L. DuBois'
_publ_contact_author_phone       '303 384 6171'
_publ_section_title
;
 [Ni(Et~2~PCH~2~NMeCH~2~PEt~2~)~2~]^2+^ as a Functional Model for
 Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              216
_journal_page_last               227
_journal_paper_doi               10.1021/ic020610v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C16 H41 B2 F8 N Ni P4'
_chemical_formula_weight         603.71
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.595(3)
_cell_length_b                   9.0279(12)
_cell_length_c                   16.339(2)
_cell_measurement_reflns_used    5850
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.709
_cell_measurement_theta_min      2.508
_cell_volume                     2742.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(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         'sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25140
_diffrn_reflns_theta_full        29.49
_diffrn_reflns_theta_max         29.49
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.7738
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta. Cryst.(1995), A51, 33-38'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(16)
_refine_ls_extinction_coef       0.0018(4)
_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_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7135
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+1.9825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                6134
_reflns_number_total             7135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020610v_1.cif
_cod_data_source_block           bc427
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312868