Syntheses and Structural Diversity of Group 2 and Group 12 Tris(pyrazolyl)methaneand Zwitterionic Tris(pyrazolyl)methanideCompounds
Cushion, Michael G.; Meyer, Jens; Heath, Alex; Schwarz, Andrew D.; Fernández, Ignacio; Breher, Frank; Mountford, Philip; Organometallics 29 (2010) 1174–; doi:10.1021/om901013b

data_4067545
_publ_section_title
;
 Syntheses and Structural Diversity of Group 2 and Group 12
 Tris(pyrazolyl)methaneand Zwitterionic Tris(pyrazolyl)methanideCompounds
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1174
_journal_paper_doi               10.1021/om901013b
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C22 H39 Mg1 N7 Si2'
_chemical_formula_sum            'C22 H39 Mg N7 Si2'
_chemical_formula_weight         482.08
_chemical_name_systematic
;
Mg{C(Me2pz)3}{N(SiMe3)2}
;
_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           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 119.5460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3849(2)
_cell_length_b                   24.5357(4)
_cell_length_c                   16.1402(2)
_cell_measurement_reflns_used    12443
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5644.82(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31644
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         5.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000774
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.943 -0.791 0.506 -0.344 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0597
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0413
_reflns_limit_h_max              18
_reflns_limit_h_min              -21
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7190
_reflns_number_total             12459
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.4111(4)
_cod_data_source_file            om901013b_si_001.cif
_cod_data_source_block           compound_13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_Hall     '-P 2yn '
_cod_original_formula_sum        'C22 H39 Mg1 N7 Si2'
_cod_database_code               4067545