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_4105707
_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_moiety         'C52 H50 Cl Ni P2 S2, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C54 H54 Cl5 F6 Ni P3 S2'
_chemical_formula_weight         1209.96
_chemical_name_systematic
; 
 ? 
;
_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-97
_audit_update_record
;
2010-04-08 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.397(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5619(10)
_cell_length_b                   19.1526(15)
_cell_length_c                   24.083(2)
_cell_measurement_reflns_used    2717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.26
_cell_measurement_theta_min      2.95
_cell_volume                     5323.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1945
_diffrn_reflns_av_sigmaI/netI    0.2470
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20294
_diffrn_reflns_theta_full        59.11
_diffrn_reflns_theta_max         59.11
_diffrn_reflns_theta_min         2.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.915
_exptl_absorpt_correction_T_max  0.8338
_exptl_absorpt_correction_T_min  0.2903
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       needle
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1907
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0991P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2447
_reflns_number_gt                3083
_reflns_number_total             7484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109624m_si_002_8.cif
_cod_data_source_block           n0275
_cod_original_cell_volume        5323.5(8)
_cod_database_code               4105707