#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/75/4067553.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4067553
loop_
_publ_author_name
'Cushion, Michael G.'
'Meyer, Jens'
'Heath, Alex'
'Schwarz, Andrew D.'
'Fernández, Ignacio'
'Breher, Frank'
'Mountford, Philip'
_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         'C26 H30 Mg1 N12'
_chemical_formula_sum            'C26 H30 Mg N12'
_chemical_formula_weight         534.91
_chemical_name_systematic
;
Mg{C(Me2pz)3}{C(pz)3}
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 94.3134(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.6839(11)
_cell_length_b                   13.3948(4)
_cell_length_c                   8.0750(3)
_cell_measurement_reflns_used    3878
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     3848.7(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3929
_diffrn_reflns_theta_full        25.534
_diffrn_reflns_theta_max         26.055
_diffrn_reflns_theta_min         5.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.923
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9881
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2762
_refine_ls_number_restraints     283
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.001765
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.27 0.943 0.787 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1035
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0817
_reflns_limit_h_max              43
_reflns_limit_h_min              -44
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                2762
_reflns_number_total             3929
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.84
_oxford_diffrn_Wilson_scale      12.20
_oxford_refine_ls_r_factor_ref   0.0787
_oxford_refine_ls_scale          0.3306(11)
_oxford_reflns_number_all        3925
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            om901013b_si_001.cif
_cod_data_source_block           compound_26
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 1 2/m 1 '
_cod_original_formula_sum        'C26 H30 Mg1 N12'
_cod_database_code               4067553
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z
x,-y,z
-x+1/2,y+1/2,-z
x+1/2,-y+1/2,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Mg1 Mg 0.35019(3) 0.0000 0.49867(12) 0.0353 1.0000 Uani S TU
N1 N 0.30085(7) 0.0000 0.3210(3) 0.0409 1.0000 Uani S TU
C1 C 0.29308(10) 0.0000 0.1573(4) 0.0429 1.0000 Uani S TU
N2 N 0.26676(7) 0.0000 0.3912(3) 0.0391 1.0000 Uani S TU
C2 C 0.25380(10) 0.000000(7) 0.1213(4) 0.0472 1.0000 Uani S TU
N3 N 0.31934(5) -0.10837(14) 0.6327(2) 0.0374 1.0000 Uani . U
C3 C 0.23799(9) 0.0000 0.2709(4) 0.0420 1.0000 Uani S TU
N4 N 0.28141(5) -0.08859(15) 0.6387(2) 0.0384 1.0000 Uani . U
C4 C 0.32296(11) 0.000000(7) 0.0389(4) 0.0554 1.0000 Uani S TU
N5 N 0.40221(7) 0.0000 0.6625(3) 0.0382 1.0000 Uani S TU
C5 C 0.19822(10) 0.000000(7) 0.3118(5) 0.0532 1.0000 Uani S TU
N6 N 0.43549(7) 0.0000 0.5860(3) 0.0372 1.0000 Uani S TU
C6 C 0.32521(7) -0.19621(18) 0.7086(3) 0.0439 1.0000 Uani . U
N7 N 0.38114(5) -0.10800(15) 0.3608(2) 0.0420 1.0000 Uani . U
C7 C 0.29161(7) -0.2334(2) 0.7626(3) 0.0507 1.0000 Uani . U
N8 N 0.41825(5) -0.08746(14) 0.3397(2) 0.0389 1.0000 Uani . U
C8 C 0.26442(7) -0.1644(2) 0.7156(3) 0.0464 1.0000 Uani . U
C9 C 0.36335(8) -0.2420(2) 0.7283(4) 0.0570 1.0000 Uani . U
C10 C 0.22289(8) -0.1675(3) 0.7329(4) 0.0616 1.0000 Uani . U
C11 C 0.26318(9) 0.0000 0.5679(4) 0.0400 1.0000 Uani S TU
C12 C 0.41214(9) 0.000000(7) 0.8232(4) 0.0457 1.0000 Uani S TU
C13 C 0.45098(10) 0.000000(7) 0.8538(5) 0.0543 1.0000 Uani S TU
C14 C 0.46483(9) 0.000000(7) 0.7011(4) 0.0465 1.0000 Uani S TU
C15 C 0.37400(8) -0.1930(2) 0.2785(3) 0.0536 1.0000 Uani . U
C16 C 0.40548(9) -0.2279(2) 0.2050(4) 0.0637 1.0000 Uani . U
C17 C 0.43281(7) -0.1590(2) 0.2460(3) 0.0506 1.0000 Uani . U
C18 C 0.43787(8) 0.0000 0.4077(4) 0.0389 1.0000 Uani S TU
H21 H 0.2406 0.0000 0.0152 0.0561 1.0000 Uiso RS .
H71 H 0.2887 -0.2952 0.8193 0.0611 1.0000 Uiso R .
H91 H 0.3790 -0.2174 0.6446 0.0874 1.0000 Uiso R .
H92 H 0.3745 -0.2235 0.8343 0.0877 1.0000 Uiso R .
H93 H 0.3621 -0.3148 0.7238 0.0877 1.0000 Uiso R .
H101 H 0.2103 -0.1955 0.6332 0.0930 1.0000 Uiso R .
H102 H 0.2177 -0.2087 0.8250 0.0930 1.0000 Uiso R .
H103 H 0.2130 -0.1004 0.7492 0.0932 1.0000 Uiso R .
H121 H 0.3953 0.0000 0.9059 0.0528 1.0000 Uiso RS .
H131 H 0.4648 0.0000 0.9558 0.0639 1.0000 Uiso RS .
H141 H 0.4895 0.0000 0.6783 0.0539 1.0000 Uiso RS .
H151 H 0.3512 -0.2252 0.2719 0.0639 1.0000 Uiso R .
H161 H 0.4077 -0.2855 0.1423 0.0750 1.0000 Uiso R .
H171 H 0.4577 -0.1611 0.2153 0.0594 1.0000 Uiso R .
H51 H 0.1828 0.0000 0.2082 0.0800 1.0000 Uiso RS .
H52 H 0.1933 0.0596 0.3757 0.0801 1.0000 Uiso R .
H41 H 0.3470 0.0000 0.0978 0.0850 1.0000 Uiso RS .
H42 H 0.3202 -0.0580 -0.0303 0.0852 1.0000 Uiso R .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mg 0.0486 0.0363 5.4204 2.8275 2.1735 79.2611 1.2269 0.3808 2.3073 7.1937
0.8584 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 6_555 Mg1 N7 6_555 96.14(7) yes
N3 6_555 Mg1 N1 . 85.03(7) yes
N7 6_555 Mg1 N1 . 94.52(8) yes
N3 6_555 Mg1 N3 . 84.40(10) yes
N7 6_555 Mg1 N3 . 179.27(9) yes
N1 . Mg1 N3 . 85.03(7) yes
N3 6_555 Mg1 N5 . 97.90(8) yes
N7 6_555 Mg1 N5 . 82.52(8) yes
N1 . Mg1 N5 . 176.02(10) yes
N3 . Mg1 N5 . 97.90(8) yes
N3 6_555 Mg1 N7 . 179.27(9) yes
N7 6_555 Mg1 N7 . 83.31(11) yes
N1 . Mg1 N7 . 94.52(8) yes
N3 . Mg1 N7 . 96.14(7) yes
N5 . Mg1 N7 . 82.52(8) yes
Mg1 . N1 C1 . 138.6(2) yes
Mg1 . N1 N2 . 114.92(19) yes
C1 . N1 N2 . 106.5(3) yes
N1 . C1 C2 . 109.6(3) yes
N1 . C1 C4 . 122.3(3) yes
C2 . C1 C4 . 128.1(3) yes
N1 . N2 C3 . 110.4(3) yes
N1 . N2 C11 . 123.6(2) yes
C3 . N2 C11 . 126.1(3) yes
C1 . C2 C3 . 106.7(3) yes
C1 . C2 H21 . 127.4 no
C3 . C2 H21 . 126.0 no
Mg1 . N3 N4 . 115.17(14) yes
Mg1 . N3 C6 . 138.88(16) yes
N4 . N3 C6 . 105.82(18) yes
C2 . C3 N2 . 106.9(3) yes
C2 . C3 C5 . 131.4(3) yes
N2 . C3 C5 . 121.7(3) yes
N3 . N4 C8 . 110.16(19) yes
N3 . N4 C11 . 123.64(19) yes
C8 . N4 C11 . 126.2(2) yes
C1 . C4 H42 6_555 109.2 no
C1 . C4 H41 . 110.1 no
H42 6_555 C4 H41 . 109.9 no
C1 . C4 H42 . 109.2 no
H42 6_555 C4 H42 . 108.5 no
H41 . C4 H42 . 109.9 no
Mg1 . N5 N6 . 116.55(19) yes
Mg1 . N5 C12 . 138.1(2) yes
N6 . N5 C12 . 105.3(2) yes
C3 . C5 H52 6_555 109.4 no
C3 . C5 H51 . 107.3 no
H52 6_555 C5 H51 . 110.2 no
C3 . C5 H52 . 109.4 no
H52 6_555 C5 H52 . 110.2 no
H51 . C5 H52 . 110.2 no
N5 . N6 C14 . 110.0(3) yes
N5 . N6 C18 . 124.2(2) yes
C14 . N6 C18 . 125.8(3) yes
N3 . C6 C7 . 110.4(2) yes
N3 . C6 C9 . 121.5(2) yes
C7 . C6 C9 . 128.1(2) yes
Mg1 . N7 N8 . 117.43(14) yes
Mg1 . N7 C15 . 137.50(17) yes
N8 . N7 C15 . 105.00(19) yes
C6 . C7 C8 . 106.2(2) yes
C6 . C7 H71 . 125.8 no
C8 . C7 H71 . 128.0 no
N7 . N8 C17 . 110.02(19) yes
N7 . N8 C18 . 123.77(19) yes
C17 . N8 C18 . 126.2(2) yes
C7 . C8 N4 . 107.4(2) yes
C7 . C8 C10 . 129.7(2) yes
N4 . C8 C10 . 122.8(2) yes
C6 . C9 H91 . 110.9 no
C6 . C9 H92 . 107.8 no
H91 . C9 H92 . 108.4 no
C6 . C9 H93 . 111.6 no
H91 . C9 H93 . 110.0 no
H92 . C9 H93 . 108.0 no
C8 . C10 H101 . 109.4 no
C8 . C10 H102 . 109.9 no
H101 . C10 H102 . 108.5 no
C8 . C10 H103 . 110.9 no
H101 . C10 H103 . 108.6 no
H102 . C10 H103 . 109.4 no
N4 6_555 C11 N4 . 109.9(2) yes
N4 6_555 C11 N2 . 108.64(17) yes
N4 . C11 N2 . 108.64(17) yes
N5 . C12 C13 . 111.4(3) yes
N5 . C12 H121 . 124.4 no
C13 . C12 H121 . 124.2 no
C12 . C13 C14 . 105.3(3) yes
C12 . C13 H131 . 127.9 no
C14 . C13 H131 . 126.8 no
C13 . C14 N6 . 108.0(3) yes
C13 . C14 H141 . 127.1 no
N6 . C14 H141 . 124.9 no
N7 . C15 C16 . 111.7(2) yes
N7 . C15 H151 . 124.4 no
C16 . C15 H151 . 123.9 no
C15 . C16 C17 . 104.7(2) yes
C15 . C16 H161 . 127.9 no
C17 . C16 H161 . 127.3 no
C16 . C17 N8 . 108.5(2) yes
C16 . C17 H171 . 126.0 no
N8 . C17 H171 . 125.4 no
N8 . C18 N8 6_555 107.6(2) yes
N8 . C18 N6 . 108.29(16) yes
N8 6_555 C18 N6 . 108.29(16) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mg1 N3 6_555 2.1609(19) yes
Mg1 N7 6_555 2.177(2) yes
Mg1 N1 . 2.186(3) yes
Mg1 N3 . 2.1609(19) yes
Mg1 N5 . 2.197(3) yes
Mg1 N7 . 2.177(2) yes
N1 C1 . 1.329(4) yes
N1 N2 . 1.380(4) yes
C1 C2 . 1.410(5) yes
C1 C4 . 1.485(5) yes
N2 C3 . 1.360(4) yes
N2 C11 . 1.442(4) yes
C2 C3 . 1.371(5) yes
C2 H21 . 0.946 no
N3 N4 . 1.384(2) yes
N3 C6 . 1.336(3) yes
C3 C5 . 1.481(5) yes
N4 C8 . 1.356(3) yes
N4 C11 . 1.450(3) yes
C4 H42 6_555 0.958 no
C4 H41 . 0.951 no
C4 H42 . 0.958 no
N5 N6 . 1.379(3) yes
N5 C12 . 1.319(4) yes
C5 H52 6_555 0.974 no
C5 H51 . 0.965 no
C5 H52 . 0.974 no
N6 C14 . 1.347(4) yes
N6 C18 . 1.448(4) yes
C6 C7 . 1.398(3) yes
C6 C9 . 1.490(4) yes
N7 N8 . 1.376(3) yes
N7 C15 . 1.333(3) yes
C7 C8 . 1.373(4) yes
C7 H71 . 0.955 no
N8 C17 . 1.349(3) yes
N8 C18 . 1.451(3) yes
C8 C10 . 1.499(3) yes
C9 H91 . 0.967 no
C9 H92 . 0.950 no
C9 H93 . 0.976 no
C10 H101 . 0.968 no
C10 H102 . 0.957 no
C10 H103 . 0.978 no
C12 C13 . 1.389(5) yes
C12 H121 . 0.932 no
C13 C14 . 1.362(5) yes
C13 H131 . 0.928 no
C14 H141 . 0.914 no
C15 C16 . 1.391(4) yes
C15 H151 . 0.920 no
C16 C17 . 1.365(4) yes
C16 H161 . 0.929 no
C17 H171 . 0.941 no
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.040 673 85 ' '
2 0.500 0.500 0.026 673 85 ' '
