Mononuclear (O,O′ orN,N′) and Heterodinuclear (O,O′ andN,N′) Transition-Metal Complexes ofortho-Quinoid Bis(pyrazol-1-yl)methane Ligands
Blasberg, Florian; Bolte, Michael; Lerner, Hans-Wolfram; Wagner, Matthias; Organometallics 31 (2012) 3213–; doi:10.1021/om3000746

data_4078060
_publ_section_title
;
 Mononuclear (O,O&#x2032; orN,N&#x2032;) and Heterodinuclear (O,O&#x2032;
 andN,N&#x2032;) Transition-Metal Complexes ofortho-Quinoid
 Bis(pyrazol-1-yl)methane Ligands
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3213
_journal_paper_doi               10.1021/om3000746
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C30 H40 N5 O2, N O3, 1.5(H2 O)'
_chemical_formula_sum            'C30 H43 N6 O6.5'
_chemical_formula_weight         591.70
_chemical_name_systematic        ?
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   34.6611(4)
_cell_length_b                   34.6611(4)
_cell_length_c                   22.3350(3)
_cell_measurement_reflns_used    172686
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      67.66
_cell_measurement_theta_min      2.36
_cell_volume                     26833.1(6)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_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  0.1571
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            244174
_diffrn_reflns_theta_full        63.68
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             10144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.531
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00029(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   1.533
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         11025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.533
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.1109
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3432
_refine_ls_wR_factor_ref         0.3694
_reflns_number_gt                7870
_reflns_number_total             11025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om3000746_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      I41/a
_cod_original_formula_sum        'C30 H43 N6 O6.50'
_cod_database_code               4078060