Sodium, magnesium and zinc complexes of mono(phenolate) heteroscorpionate ligands
Schofield, A. Daniel; Barros, Mariana Luna; Cushion, Michael G.; Schwarz, Andrew D.; Mountford, Philip; Dalton Transactions  (2009) 85–96; doi:10.1039/b813116c

data_7000206
_publ_section_title
;
 Sodium, magnesium and zinc complexes of mono(phenolate)
 heteroscorpionate ligands
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              85
_journal_page_last               96
_journal_paper_doi               10.1039/b813116c
_journal_year                    2009
_chemical_formula_moiety         'C31 H53 Mg1 N5 O1 Si2, 0.5(C7 H8)'
_chemical_formula_sum            'C34.5 H57 Mg N5 O Si2'
_chemical_formula_weight         638.34
_chemical_name_common            Mg((Me2pz)2C(C6H2(tBu)2O)(N(SiMe3)2)
_chemical_name_systematic
;
Mg{(Me2pz)2C(C6H2(tBu)2O}{N(SiMe3)2}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.6153(10)
_cell_angle_beta                 104.8024(9)
_cell_angle_gamma                95.2213(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5864(2)
_cell_length_b                   12.7632(2)
_cell_length_c                   14.2935(3)
_cell_measurement_reflns_used    7897
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1938.95(6)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.034
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15046
_diffrn_reflns_theta_full        26.106
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         5.148
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       plate
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.55
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4887
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.009587
_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:
0.912 0.331 0.594 0.149E-02 0.141
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1027
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0704
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4887
_reflns_number_total             8798
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.68
_oxford_diffrn_Wilson_scale      4.86
_oxford_refine_ls_scale          0.4686(10)
_cod_data_source_file            b813116c.txt
_cod_data_source_block           compound_6.0.5(C7H8)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C34.50 H57 Mg1 N5 O1 Si2'
_cod_database_code               7000206