Plasticity of the Nickel(II) Coordination Environment in Complexes with Hemilabile Phosphino Thioether Ligands
Charles W. Machan; Alexander M. Spokoyny; Matthew R. Jones; Amy A. Sarjeant; Charlotte L. Stern; Chad A. Mirkin; Journal of the American Chemical Society 133 (2011) 3023–3033; doi:10.1021/ja109624m

data_4105701
_publ_contact_author_address
;
Department of Chemistry and the International Institute for Nanotechnology, 
Northwestern University, 2145 Sheridan Road, Evanston, IL, 60208, USA.
;
_publ_contact_author_email       chadnano@northwestern.edu
_publ_contact_author_fax         847-467-5123
_publ_contact_author_name        'Chad A. Mirkin'
_publ_section_title
;
 Plasticity of the Nickel(II) Coordination Environment in Complexes with
 Hemilabile Phosphino Thioether Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3023
_journal_page_last               3033
_journal_paper_doi               10.1021/ja109624m
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C32 H36 Cl6 Ni O8 P2 S2'
_chemical_formula_weight         946.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-04-08 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.7670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.9346(6)
_cell_length_b                   13.1360(3)
_cell_length_c                   25.7007(8)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.23
_cell_measurement_theta_min      3.71
_cell_volume                     8046.1(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27233
_diffrn_reflns_theta_full        64.67
_diffrn_reflns_theta_max         64.67
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    6.486
_exptl_absorpt_correction_T_max  0.6249
_exptl_absorpt_correction_T_min  0.2440
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       tabular
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6699
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1055P)^2^+31.3930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                5572
_reflns_number_total             6699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109624m_si_002_2.cif
_cod_data_source_block           n0117
_cod_database_code               4105701