#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:33:29 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224283 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/85/7048532.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_7048532
loop_
_publ_author_name
'Luna Barros, Mariana'
'Cushion, Michael G.'
'Schwarz, Andrew D.'
'Turner, Zoë R'
'Mountford, Philip'
_publ_section_title
;
 Magnesium, calcium and zinc [N₂N'] heteroscorpionate
 complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4124
_journal_page_last               4138
_journal_paper_doi               10.1039/c8dt04985h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H50 Mg1 N6 Si3'
_chemical_formula_sum            'C22 H50 Mg N6 Si3'
_chemical_formula_weight         507.24
_chemical_name_systematic
;
 Mg{(Me2pz)2CHSiMe2NiPr}({N(SiMe3)2}
;
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-12-18 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6864(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3686(2)
_cell_length_b                   13.7276(4)
_cell_length_c                   11.7088(3)
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1526.19(7)
_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 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6618
_diffrn_reflns_theta_full        26.394
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         5.222
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1675
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2428
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.002660
_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: 
 1.34 0.745 1.16 0.194 0.309 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0746
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0607
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                2428
_reflns_number_total             3604
_reflns_threshold_expression     I>3.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.03
_oxford_diffrn_Wilson_scale      3.04
_oxford_refine_ls_scale          0.6011(18)
_cod_data_source_file            c8dt04985h2.cif
_cod_data_source_block           compound17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048527--7048538.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/m 1 '
_cod_original_formula_sum        'C22 H50 Mg1 N6 Si3'
_cod_database_code               7048532
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z
x,-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 -0.18258(12) 0.7500 0.19961(11) 0.0208 1.0000 Uani S T
N1 N -0.0280(2) 0.86073(18) 0.21938(19) 0.0251 1.0000 Uani . .
N2 N 0.1059(2) 0.83704(18) 0.3007(2) 0.0257 1.0000 Uani . .
N3 N -0.1549(3) 0.7500 0.3805(3) 0.0319 1.0000 Uani DS TU
N4 N -0.3500(3) 0.7500 0.0357(3) 0.0239 1.0000 Uani S T
Si1 Si 0.01558(11) 0.7500 0.47761(9) 0.0248 1.0000 Uani S T
Si2 Si -0.50881(11) 0.7500 0.04793(10) 0.0270 1.0000 Uani S T
Si3 Si -0.33443(11) 0.7500 -0.10370(9) 0.0241 1.0000 Uani S T
C1 C -0.0196(3) 0.9495(2) 0.1773(2) 0.0281 1.0000 Uani . .
C2 C 0.1198(3) 0.9837(2) 0.2327(3) 0.0356 1.0000 Uani . .
C3 C 0.1966(3) 0.9112(2) 0.3109(3) 0.0322 1.0000 Uani . .
C4 C -0.1473(3) 1.0000(2) 0.0863(3) 0.0389 1.0000 Uani . .
C5 C 0.3497(3) 0.9062(3) 0.3959(3) 0.0457 1.0000 Uani . .
C6 C 0.1251(4) 0.750000(8) 0.3764(3) 0.0236 1.0000 Uani S T
C7 C 0.0898(3) 0.8603(3) 0.5767(3) 0.0429 1.0000 Uani . .
C8 C -0.2671(4) 0.750001(8) 0.4256(4) 0.0637 1.0000 Uani DS TU
C9 C -0.2660(9) 0.8514(3) 0.4791(8) 0.0767 0.5000 Uani D U
C91 C -0.2575(9) 0.6891(7) 0.5365(6) 0.0759 0.5000 Uani D U
C10 C -0.5270(4) 0.8614(3) 0.1324(4) 0.0511 1.0000 Uani . .
C11 C -0.6703(5) 0.750000(8) -0.1006(4) 0.0493 1.0000 Uani S T
C12 C -0.4167(3) 0.6415(3) -0.2057(3) 0.0358 1.0000 Uani . .
C13 C -0.1438(4) 0.750000(8) -0.0804(4) 0.0309 1.0000 Uani S T
H21 H 0.1557 1.0480 0.2179 0.0444 1.0000 Uiso R .
H41 H -0.1327 1.0179 0.0095 0.0450 1.0000 Uiso R .
H42 H -0.2310 0.9561 0.0633 0.0450 1.0000 Uiso R .
H43 H -0.1643 1.0605 0.1257 0.0450 1.0000 Uiso R .
H51 H 0.3969 0.9681 0.3890 0.0533 1.0000 Uiso R .
H52 H 0.3602 0.8973 0.4840 0.0533 1.0000 Uiso R .
H53 H 0.3942 0.8501 0.3710 0.0533 1.0000 Uiso R .
H61 H 0.2262 0.7500 0.4362 0.0284 1.0000 Uiso RS .
H71 H 0.1921 0.8499 0.6295 0.0513 1.0000 Uiso R .
H72 H 0.0383 0.8718 0.6317 0.0513 1.0000 Uiso R .
H73 H 0.0784 0.9182 0.5217 0.0513 1.0000 Uiso R .
H91 H -0.3428 0.8558 0.5099 0.0902 0.5000 Uiso R .
H92 H -0.2812 0.9019 0.4134 0.0902 0.5000 Uiso R .
H93 H -0.1730 0.8626 0.5500 0.0902 0.5000 Uiso R .
H101 H -0.6202 0.8606 0.1389 0.0656 1.0000 Uiso R .
H102 H -0.5204 0.9206 0.0853 0.0656 1.0000 Uiso R .
H103 H -0.4498 0.8628 0.2180 0.0656 1.0000 Uiso R .
H111 H -0.7563 0.7500 -0.0819 0.0619 1.0000 Uiso RS .
H112 H -0.6702 0.8095 -0.1499 0.0619 1.0000 Uiso R .
H113 H -0.6702 0.6905 -0.1499 0.0619 1.0000 Uiso R .
H121 H -0.4030 0.6468 -0.2853 0.0437 1.0000 Uiso R .
H122 H -0.5198 0.6396 -0.2248 0.0437 1.0000 Uiso R .
H123 H -0.3711 0.5804 -0.1611 0.0437 1.0000 Uiso R .
H131 H -0.1372 0.7500 -0.1632 0.0399 1.0000 Uiso RS .
H132 H -0.0965 0.8095 -0.0326 0.0399 1.0000 Uiso R .
H133 H -0.0965 0.6905 -0.0326 0.0399 1.0000 Uiso R .
H911 H -0.3407 0.7006 0.5574 0.0915 0.5000 Uiso R .
H912 H -0.1690 0.7037 0.6110 0.0915 0.5000 Uiso R .
H913 H -0.2565 0.6195 0.5115 0.0915 0.5000 Uiso R .
H81 H -0.3597 0.7500 0.3544 0.0771 1.0000 Uiso RS .
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'
Si 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 '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
N1 4_565 Mg1 N1 . 89.84(13) yes
N1 4_565 Mg1 N3 . 95.81(9) yes
N1 . Mg1 N3 . 95.81(9) yes
N1 4_565 Mg1 N4 . 115.07(9) yes
N1 . Mg1 N4 . 115.07(9) yes
N3 . Mg1 N4 . 135.02(14) yes
Mg1 . N1 N2 . 114.19(17) yes
Mg1 . N1 C1 . 139.81(19) yes
N2 . N1 C1 . 106.0(2) yes
N1 . N2 C3 . 110.8(2) yes
N1 . N2 C6 . 118.1(2) yes
C3 . N2 C6 . 130.0(2) yes
Mg1 . N3 Si1 . 112.24(15) yes
Mg1 . N3 C8 . 125.6(3) yes
Si1 . N3 C8 . 122.2(3) yes
Mg1 . N4 Si2 . 114.36(17) yes
Mg1 . N4 Si3 . 122.56(18) yes
Si2 . N4 Si3 . 123.08(18) yes
C7 4_565 Si1 N3 . 118.65(12) yes
C7 4_565 Si1 C6 . 100.51(13) yes
N3 . Si1 C6 . 107.59(15) yes
C7 4_565 Si1 C7 . 107.7(2) yes
N3 . Si1 C7 . 118.65(12) yes
C6 . Si1 C7 . 100.51(13) yes
C10 4_565 Si2 N4 . 110.44(14) yes
C10 4_565 Si2 C10 . 109.6(3) yes
N4 . Si2 C10 . 110.44(14) yes
C10 4_565 Si2 C11 . 104.44(15) yes
N4 . Si2 C11 . 117.07(19) yes
C10 . Si2 C11 . 104.44(15) yes
C12 4_565 Si3 N4 . 114.45(12) yes
C12 4_565 Si3 C12 . 104.4(2) yes
N4 . Si3 C12 . 114.45(12) yes
C12 4_565 Si3 C13 . 105.86(13) yes
N4 . Si3 C13 . 111.04(17) yes
C12 . Si3 C13 . 105.86(13) yes
N1 . C1 C2 . 110.1(3) yes
N1 . C1 C4 . 121.1(3) yes
C2 . C1 C4 . 128.8(3) yes
C1 . C2 C3 . 106.2(3) yes
C1 . C2 H21 . 126.9 no
C3 . C2 H21 . 126.9 no
C2 . C3 N2 . 106.8(3) yes
C2 . C3 C5 . 130.8(3) yes
N2 . C3 C5 . 122.4(3) yes
C1 . C4 H41 . 110.1 no
C1 . C4 H42 . 109.7 no
H41 . C4 H42 . 109.5 no
C1 . C4 H43 . 109.0 no
H41 . C4 H43 . 109.2 no
H42 . C4 H43 . 109.2 no
C3 . C5 H51 . 109.2 no
C3 . C5 H52 . 109.8 no
H51 . C5 H52 . 109.5 no
C3 . C5 H53 . 109.4 no
H51 . C5 H53 . 109.5 no
H52 . C5 H53 . 109.5 no
N2 . C6 N2 4_565 110.6(3) yes
N2 . C6 Si1 . 113.68(18) yes
N2 4_565 C6 Si1 . 113.68(18) yes
N2 . C6 H61 . 106.0 no
N2 4_565 C6 H61 . 106.0 no
Si1 . C6 H61 . 106.1 no
Si1 . C7 H71 . 109.7 no
Si1 . C7 H72 . 109.4 no
H71 . C7 H72 . 109.5 no
Si1 . C7 H73 . 109.3 no
H71 . C7 H73 . 109.5 no
H72 . C7 H73 . 109.5 no
C9 4_565 C8 N3 . 105.9(4) yes
C91 4_565 C8 N3 . 121.6(4) yes
N3 . C8 C9 . 105.9(4) yes
N3 . C8 C91 . 121.6(4) yes
C9 . C8 C91 . 99.5(7) yes
C9 4_565 C8 H81 . 101.0 no
C91 4_565 C8 H81 . 115.5 no
N3 . C8 H81 . 109.9 no
C9 . C8 H81 . 101.0 no
C91 . C8 H81 . 115.5 no
C8 . C9 H91 . 109.1 no
C8 . C9 H92 . 110.2 no
H91 . C9 H92 . 109.5 no
C8 . C9 H93 . 109.1 no
H91 . C9 H93 . 109.5 no
H92 . C9 H93 . 109.5 no
H93 4_565 C91 C8 . 104.9 no
H93 4_565 C91 H91 4_565 101.6 no
C8 . C91 H91 4_565 108.8 no
H93 4_565 C91 H911 . 142.3 no
C8 . C91 H911 . 110.9 no
H91 4_565 C91 H911 . 56.0 no
H93 4_565 C91 H912 . 66.5 no
C8 . C91 H912 . 111.1 no
H91 4_565 C91 H912 . 140.1 no
H911 . C91 H912 . 109.5 no
H93 4_565 C91 H913 . 47.0 no
C8 . C91 H913 . 106.4 no
H91 4_565 C91 H913 . 56.1 no
H911 . C91 H913 . 109.5 no
H912 . C91 H913 . 109.5 no
Si2 . C10 H101 . 109.7 no
Si2 . C10 H102 . 109.2 no
H101 . C10 H102 . 109.5 no
Si2 . C10 H103 . 109.5 no
H101 . C10 H103 . 109.5 no
H102 . C10 H103 . 109.5 no
H113 4_565 C11 H112 4_565 109.5 no
H113 4_565 C11 Si2 . 109.2 no
H112 4_565 C11 Si2 . 109.2 no
H113 4_565 C11 H111 . 109.5 no
H112 4_565 C11 H111 . 109.5 no
Si2 . C11 H111 . 109.9 no
H112 4_565 C11 H112 . 109.5 no
Si2 . C11 H112 . 109.2 no
H111 . C11 H112 . 109.5 no
H113 4_565 C11 H113 . 109.5 no
Si2 . C11 H113 . 109.2 no
H111 . C11 H113 . 109.5 no
H112 . C11 H113 . 109.5 no
Si3 . C12 H121 . 109.6 no
Si3 . C12 H122 . 109.4 no
H121 . C12 H122 . 109.5 no
Si3 . C12 H123 . 109.4 no
H121 . C12 H123 . 109.5 no
H122 . C12 H123 . 109.5 no
H133 4_565 C13 H132 4_565 109.5 no
H133 4_565 C13 Si3 . 109.4 no
H132 4_565 C13 Si3 . 109.4 no
H133 4_565 C13 H131 . 109.5 no
H132 4_565 C13 H131 . 109.5 no
Si3 . C13 H131 . 109.7 no
H132 4_565 C13 H132 . 109.5 no
Si3 . C13 H132 . 109.4 no
H131 . C13 H132 . 109.5 no
H133 4_565 C13 H133 . 109.5 no
Si3 . C13 H133 . 109.4 no
H131 . C13 H133 . 109.5 no
H132 . C13 H133 . 109.5 no
C91 4_565 H91 C9 . 49.7 no
C91 4_565 H93 C9 . 47.7 no
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 N1 4_565 2.153(2) yes
Mg1 N1 . 2.153(2) yes
Mg1 N3 . 2.020(3) yes
Mg1 N4 . 2.005(3) yes
N1 N2 . 1.370(3) yes
N1 C1 . 1.331(4) yes
N2 C3 . 1.359(4) yes
N2 C6 . 1.453(3) yes
N3 Si1 . 1.674(3) yes
N3 C8 . 1.457(2) yes
N4 Si2 . 1.709(3) yes
N4 Si3 . 1.703(3) yes
Si1 C7 4_565 1.875(3) yes
Si1 C6 . 1.943(4) yes
Si1 C7 . 1.875(3) yes
Si2 C10 4_565 1.872(4) yes
Si2 C10 . 1.872(4) yes
Si2 C11 . 1.868(4) yes
Si3 C12 4_565 1.886(3) yes
Si3 C12 . 1.886(3) yes
Si3 C13 . 1.884(4) yes
C1 C2 . 1.405(4) yes
C1 C4 . 1.495(4) yes
C2 C3 . 1.370(5) yes
C2 H21 . 1.000 no
C3 C5 . 1.498(4) yes
C4 H41 . 1.000 no
C4 H42 . 1.000 no
C4 H43 . 1.000 no
C5 H51 . 1.000 no
C5 H52 . 1.000 no
C5 H53 . 1.000 no
C6 H61 . 1.000 no
C7 H71 . 1.000 no
C7 H72 . 1.000 no
C7 H73 . 1.000 no
C8 C9 . 1.525(2) yes
C8 C91 . 1.514(2) yes
C8 H81 . 0.987 no
C9 H91 . 1.000 no
C9 H92 . 1.000 no
C9 H93 . 1.000 no
C91 H93 4_565 1.088 no
C91 H91 4_565 1.019 no
C91 H911 . 1.000 no
C91 H912 . 1.000 no
C91 H913 . 1.000 no
C10 H101 . 1.000 no
C10 H102 . 1.000 no
C10 H103 . 1.000 no
C11 H113 4_565 1.000 no
C11 H112 4_565 1.000 no
C11 H111 . 1.000 no
C11 H112 . 1.000 no
C11 H113 . 1.000 no
C12 H121 . 1.000 no
C12 H122 . 1.000 no
C12 H123 . 1.000 no
C13 H133 4_565 1.000 no
C13 H132 4_565 1.000 no
C13 H131 . 1.000 no
C13 H132 . 1.000 no
C13 H133 . 1.000 no
