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_4105708
_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 Ni P2 S2, 2(C F3 O3 S)'
_chemical_formula_sum            'C54 H50 F6 Ni O6 P2 S4'
_chemical_formula_weight         1157.83
_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                 99.1350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7062(2)
_cell_length_b                   21.7494(3)
_cell_length_c                   15.8611(2)
_cell_measurement_reflns_used    9174
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.20
_cell_volume                     5349.44(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88415
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.8272
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.97
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.59
_refine_diff_density_max         1.725
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         15444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+7.0885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                11905
_reflns_number_total             15444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109624m_si_002_9.cif
_cod_data_source_block           n0295a
_cod_database_code               4105708