First-Row Transition-Metal Complexes of a New Pentadentate Ligand, α,α,α',α'-Tetra(pyrazolyl)lutidine
Tyler J. Morin; Brian Bennett; Sergey V. Lindeman; James R. Gardinier; Inorganic Chemistry 47 (2008) 7468–7470; doi:10.1021/ic801093q

data_4306170
_publ_section_title
;
First-Row Transition-Metal Complexes of a New Pentadentate Ligand,
\a,\a,\a',\a'-Tetra(pyrazolyl)lutidine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7468
_journal_page_last               7470
_journal_paper_doi               10.1021/ic801093q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C20 H19 Cl4 Mn N9'
_chemical_formula_weight         582.18
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.000(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5304(6)
_cell_length_b                   19.2722(10)
_cell_length_c                   11.9444(6)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66
_cell_measurement_theta_min      4
_cell_volume                     2424.0(2)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19112
_diffrn_reflns_theta_full        67.20
_diffrn_reflns_theta_max         67.20
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    8.734
_exptl_absorpt_correction_T_max  0.2614
_exptl_absorpt_correction_T_min  0.1727
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical (based on real shape of the crystal) absorption
 correction followed by:
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+9.6620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                4043
_reflns_number_total             4152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801093q_si_002_1.cif
_cod_data_source_block           MnClpz4lut_gard3qa
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4306170