Exploring the limits of redox non-innocence: pseudo square planar [{κ4-Me2C(CH2NCHpy)2}Ni]n (n = 2+, 1+, 0, −1, −2) favor Ni(ii)
Williams, Valerie A.; Hulley, Elliott B.; Wolczanski, Peter T.; Lancaster, Kyle M.; Lobkovsky, Emil B.; Chemical Science 4 (2013) 3636–; doi:10.1039/c3sc50743b

data_1514786
_publ_section_title
;
 Exploring the limits of redox non-innocence: pseudo square planar
 [{\k4-Me2C(CH2N&#xE001;CHpy)2}Ni]n (n = 2+, 1+, 0, &#x2212;1, &#x2212;2)
 favor Ni(ii)
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3636
_journal_paper_doi               10.1039/c3sc50743b
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C21 H26 N6 Ni, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C23 H29 F12 N7 Ni P2'
_chemical_formula_weight         752.18
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 107.3500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2230(4)
_cell_length_b                   23.7522(8)
_cell_length_c                   15.2139(6)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.34
_cell_measurement_theta_min      2.47
_cell_volume                     3181.2(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0143
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15695
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.7935
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          2.966
_refine_ls_shift/su_mean         0.188
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.4646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                7539
_reflns_number_total             7932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc50743b.txt
_cod_data_source_block           vw11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1514786