The Role of the Second Coordination Sphere of [Ni(PCy2NBz2)2](BF4)2 in Reversible Carbon Monoxide Binding
Aaron D. Wilson; Kendra Fraze; Brendan Twamley; Susie M. Miller; Daniel L. DuBois; M. Rakowski DuBois; Journal of the American Chemical Society 130 (2008) 1061–1068; doi:10.1021/ja077328d

data_4107328
_publ_section_title
;
 The Role of the Second Coordination Sphere of [Ni(PCy2NBz2)2](BF4)2 in
 Reversible Carbon Monoxide Binding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1061
_journal_page_last               1068
_journal_paper_doi               10.1021/ja077328d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C61 H88 N4 Ni O P4, 4(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C65 H96 B2 Cl8 F8 N4 Ni O P4'
_chemical_formula_weight         1589.27
_chemical_name_common            '[RNiCO][BF4]2 + 4DCM'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   12.5244(6)
_cell_length_b                   18.3649(8)
_cell_length_c                   32.6093(15)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.30
_cell_volume                     7500.4(6)
_computing_cell_refinement       'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_data_collection       'SMART v. 5.632 (Bruker, 2006)'
_computing_data_reduction        'SAINT+  v. 7.23a (Bruker, 2006)'
_computing_molecular_graphics    'XP, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_publication_material  'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)'
_computing_structure_refinement  'XL, SHELXTL  v. 6.14 (Bruker, 2003)'
_computing_structure_solution    'XS, SHELXTL  v. 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            108875
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.6979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         13558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0703P)^2^+5.7251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                12474
_reflns_number_total             13558
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja077328d-file001.cif
_cod_data_source_block           bt1157
_cod_database_code               4107328