#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/28/2012878.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012878
loop_
_publ_author_name
'Strohmann, Carsten'
'Schildbach, Daniel'
_publ_section_title
;
 Bis{[diphenyl(piperidinomethyl)silyl]methyl}cadmium and -magnesium
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m447
_journal_page_last               m449
_journal_paper_doi               10.1107/S0108270102011307
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mg (C19 H24 N Si)2]'
_chemical_formula_moiety         'C38 H48 Mg N2 Si2'
_chemical_formula_sum            'C38 H48 Mg N2 Si2'
_chemical_formula_weight         613.27
_chemical_name_systematic
;
Bis{[diphenyl(piperidinomethyl)silyl]methyl}magnesium
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.38(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.215(5)
_cell_length_b                   6.4100(10)
_cell_length_c                   19.576(4)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.49
_cell_volume                     3409.1(11)
_computing_cell_refinement       'CELL in IPDS'
_computing_data_collection       'EXPOSE in IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        'INTEGRATE in IPDS'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       φ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13184
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(FACEIT in IPDS; Stoe & Cie, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0760P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.109
_refine_ls_wR_factor_ref         0.115
_reflns_number_gt                2453
_reflns_number_total             3223
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd1214.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012878
_cod_database_fobs_code          2012878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mg 0.000 0.26639(13) 0.25 0.0114(2) Uani d S 1 . . Mg
Si 0.106835(15) 0.30101(8) 0.19397(3) 0.01126(16) Uani d . 1 . . Si
N 0.01175(5) 0.4755(2) 0.15982(8) 0.0112(3) Uani d . 1 . . N
C1 0.06862(6) 0.1050(3) 0.23198(11) 0.0151(4) Uani d . 1 . . C
H1A 0.0849(8) 0.030(4) 0.2727(13) 0.025(6) Uiso d . 1 . . H
H1B 0.0562(9) 0.004(4) 0.1968(15) 0.038(7) Uiso d . 1 . . H
C2 0.15775(6) 0.3975(3) 0.25555(10) 0.0147(4) Uani d . 1 . . C
C3 0.17808(7) 0.2643(3) 0.30620(12) 0.0219(5) Uani d . 1 . . C
H3 0.1655(9) 0.126(4) 0.3115(14) 0.031(7) Uiso d . 1 . . H
C4 0.21658(8) 0.3272(4) 0.35054(13) 0.0298(5) Uani d . 1 . . C
H4 0.2301(12) 0.234(5) 0.3825(19) 0.055(9) Uiso d . 1 . . H
C5 0.23613(8) 0.5251(4) 0.34560(13) 0.0297(6) Uani d . 1 . . C
H5 0.2619(9) 0.565(4) 0.3729(14) 0.029(6) Uiso d . 1 . . H
C6 0.21694(7) 0.6608(4) 0.29598(12) 0.0257(5) Uani d . 1 . . C
H6 0.2307(8) 0.792(4) 0.2914(13) 0.021(6) Uiso d . 1 . . H
C7 0.17804(7) 0.5977(3) 0.25159(12) 0.0210(5) Uani d . 1 . . C
H7 0.1645(8) 0.701(4) 0.2150(13) 0.019(6) Uiso d . 1 . . H
C8 0.13661(6) 0.2333(3) 0.11173(11) 0.0148(4) Uani d . 1 . . C
C9 0.16501(7) 0.3816(3) 0.07900(12) 0.0209(5) Uani d . 1 . . C
H9 0.1705(9) 0.523(4) 0.0991(14) 0.030(6) Uiso d . 1 . . H
C10 0.18643(8) 0.3375(4) 0.01818(13) 0.0276(5) Uani d . 1 . . C
H10 0.2041(9) 0.443(4) -0.0036(15) 0.038(7) Uiso d . 1 . . H
C11 0.18027(8) 0.1444(4) -0.01198(13) 0.0313(6) Uani d . 1 . . C
H11 0.1941(10) 0.121(5) -0.0557(16) 0.044(8) Uiso d . 1 . . H
C12 0.15285(8) -0.0050(4) 0.01893(14) 0.0350(6) Uani d . 1 . . C
H12 0.1487(11) -0.143(5) -0.0008(16) 0.048(8) Uiso d . 1 . . H
C13 0.13144(7) 0.0390(4) 0.07998(13) 0.0249(5) Uani d . 1 . . C
H13 0.1139(9) -0.070(5) 0.1035(15) 0.038(7) Uiso d . 1 . . H
C14 0.06490(6) 0.5344(3) 0.17079(11) 0.0136(4) Uani d . 1 . . C
H14A 0.0666(7) 0.634(3) 0.2090(12) 0.012(5) Uiso d . 1 . . H
H14B 0.0758(8) 0.608(4) 0.1302(14) 0.027(6) Uiso d . 1 . . H
C15 -0.01832(6) 0.6682(3) 0.14876(12) 0.0161(4) Uani d . 1 . . C
H15A -0.0059(9) 0.742(4) 0.1106(15) 0.029(7) Uiso d . 1 . . H
H15B -0.0123(7) 0.754(3) 0.1895(13) 0.013(5) Uiso d . 1 . . H
C16 -0.07239(7) 0.6180(4) 0.13404(12) 0.0205(5) Uani d . 1 . . C
H16A -0.0909(8) 0.748(4) 0.1266(13) 0.022(6) Uiso d . 1 . . H
H16B -0.0843(8) 0.558(4) 0.1744(13) 0.016(5) Uiso d . 1 . . H
C17 -0.08055(7) 0.4745(4) 0.07273(13) 0.0258(5) Uani d . 1 . . C
H17A -0.1142(10) 0.434(4) 0.0664(15) 0.039(7) Uiso d . 1 . . H
H17B -0.0723(9) 0.552(4) 0.0320(15) 0.032(7) Uiso d . 1 . . H
C18 -0.04749(7) 0.2839(4) 0.08047(13) 0.0258(5) Uani d . 1 . . C
H18A -0.0494(10) 0.188(4) 0.0388(17) 0.043(8) Uiso d . 1 . . H
H18B -0.0595(10) 0.194(4) 0.1184(16) 0.039(7) Uiso d . 1 . . H
C19 0.00582(7) 0.3456(3) 0.09699(11) 0.0184(4) Uani d . 1 . . C
H19A 0.0251(8) 0.222(4) 0.1017(12) 0.016(5) Uiso d . 1 . . H
H19B 0.0180(8) 0.429(4) 0.0565(14) 0.028(6) Uiso d . 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Mg C1 2 . 123.39(11) yes
C1 Mg N 2 2 89.60(7) yes
C1 Mg N . 2 124.81(7) no
C1 Mg N 2 . 124.81(7) yes
C1 Mg N . . 89.60(7) no
N Mg N 2 . 107.02(9) yes
C1 Mg Si 2 2 33.62(5) no
C1 Mg Si . 2 154.02(6) no
N Mg Si 2 2 60.85(4) no
N Mg Si . 2 113.83(4) no
C1 Mg Si 2 . 154.02(6) no
C1 Mg Si . . 33.62(5) no
N Mg Si 2 . 113.83(4) no
N Mg Si . . 60.85(4) no
Si Mg Si 2 . 171.99(3) no
C1 Si C2 . . 112.43(10) no
C1 Si C8 . . 118.24(9) no
C2 Si C8 . . 106.45(8) no
C1 Si C14 . . 106.79(8) no
C2 Si C14 . . 107.42(9) no
C8 Si C14 . . 104.81(9) no
C1 Si Mg . . 41.64(6) no
C2 Si Mg . . 117.08(6) no
C8 Si Mg . . 136.36(6) no
C14 Si Mg . . 65.95(6) no
C19 N C15 . . 108.19(15) no
C19 N C14 . . 108.46(14) no
C15 N C14 . . 109.23(14) no
C19 N Mg . . 107.54(12) no
C15 N Mg . . 120.30(12) no
C14 N Mg . . 102.59(11) no
Si C1 Mg . . 104.73(9) no
Si C1 H1A . . 114.6(13) no
Mg C1 H1A . . 116.1(13) no
Si C1 H1B . . 110.3(16) no
Mg C1 H1B . . 99.4(15) no
H1A C1 H1B . . 111(2) no
C3 C2 C7 . . 117.26(18) no
C3 C2 Si . . 119.86(15) no
C7 C2 Si . . 122.83(16) no
C4 C3 C2 . . 121.4(2) no
C4 C3 H3 . . 117.7(15) no
C2 C3 H3 . . 120.9(15) no
C5 C4 C3 . . 120.4(2) no
C5 C4 H4 . . 120(2) no
C3 C4 H4 . . 120(2) no
C4 C5 C6 . . 119.7(2) no
C4 C5 H5 . . 120.7(17) no
C6 C5 H5 . . 119.5(17) no
C5 C6 C7 . . 119.9(2) no
C5 C6 H6 . . 120.0(15) no
C7 C6 H6 . . 120.1(15) no
C6 C7 C2 . . 121.3(2) no
C6 C7 H7 . . 118.5(13) no
C2 C7 H7 . . 120.2(13) no
C13 C8 C9 . . 116.4(2) no
C13 C8 Si . . 123.08(16) no
C9 C8 Si . . 120.50(16) no
C10 C9 C8 . . 121.7(2) no
C10 C9 H9 . . 117.6(15) no
C8 C9 H9 . . 120.7(15) no
C11 C10 C9 . . 120.3(2) no
C11 C10 H10 . . 120.2(17) no
C9 C10 H10 . . 119.4(17) no
C10 C11 C12 . . 119.5(2) no
C10 C11 H11 . . 118.2(18) no
C12 C11 H11 . . 122.2(18) no
C11 C12 C13 . . 120.2(2) no
C11 C12 H12 . . 120.8(18) no
C13 C12 H12 . . 119.0(19) no
C12 C13 C8 . . 121.9(2) no
C12 C13 H13 . . 120.1(17) no
C8 C13 H13 . . 117.9(17) no
N C14 Si . . 113.14(12) no
N C14 H14A . . 106.0(12) no
Si C14 H14A . . 109.0(12) no
N C14 H14B . . 109.8(14) no
Si C14 H14B . . 111.2(14) no
H14A C14 H14B . . 107.5(19) no
N C15 C16 . . 111.73(16) no
N C15 H15A . . 107.9(15) no
C16 C15 H15A . . 109.7(15) no
N C15 H15B . . 106.5(13) no
C16 C15 H15B . . 113.0(12) no
H15A C15 H15B . . 108(2) no
C15 C16 C17 . . 111.94(17) no
C15 C16 H16A . . 109.3(13) no
C17 C16 H16A . . 110.4(15) no
C15 C16 H16B . . 107.5(13) no
C17 C16 H16B . . 111.6(14) no
H16A C16 H16B . . 105.8(19) no
C18 C17 C16 . . 110.51(18) no
C18 C17 H17A . . 110.6(17) no
C16 C17 H17A . . 111.3(17) no
C18 C17 H17B . . 109.2(15) no
C16 C17 H17B . . 107.8(16) no
H17A C17 H17B . . 107(2) no
C17 C18 C19 . . 111.34(19) no
C17 C18 H18A . . 113.9(16) no
C19 C18 H18A . . 109.3(15) no
C17 C18 H18B . . 108.4(15) no
C19 C18 H18B . . 109.8(16) no
H18A C18 H18B . . 104(2) no
N C19 C18 . . 112.19(16) no
N C19 H19A . . 110.7(14) no
C18 C19 H19A . . 108.7(13) no
N C19 H19B . . 109.0(15) no
C18 C19 H19B . . 108.5(13) no
H19A C19 H19B . . 107.7(19) 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
Mg C1 2 2.1816(18) no
Mg C1 . 2.1816(18) yes
Mg N 2 2.2545(17) no
Mg N . 2.2545(17) yes
Mg Si 2 3.1752(8) no
Mg Si . 3.1752(9) no
Si C1 . 1.818(2) yes
Si C2 . 1.886(2) yes
Si C8 . 1.895(2) yes
Si C14 . 1.9200(19) yes
N C19 . 1.486(3) no
N C15 . 1.490(2) no
N C14 . 1.498(2) no
C1 H1A . 1.01(3) no
C1 H1B . 0.99(3) no
C2 C3 . 1.398(3) no
C2 C7 . 1.401(3) no
C3 C4 . 1.381(3) no
C3 H3 . 0.96(3) no
C4 C5 . 1.381(4) no
C4 H4 . 0.92(3) no
C5 C6 . 1.383(4) no
C5 H5 . 0.89(3) no
C6 C7 . 1.390(3) no
C6 H6 . 0.93(2) no
C7 H7 . 1.03(2) no
C8 C13 . 1.395(3) no
C8 C9 . 1.403(3) no
C9 C10 . 1.385(3) no
C9 H9 . 1.00(3) no
C10 C11 . 1.378(4) no
C10 H10 . 0.95(3) no
C11 C12 . 1.376(4) no
C11 H11 . 0.97(3) no
C12 C13 . 1.389(3) no
C12 H12 . 0.97(3) no
C13 H13 . 0.98(3) no
C14 H14A . 0.98(2) no
C14 H14B . 0.98(3) no
C15 C16 . 1.517(3) no
C15 H15A . 0.96(3) no
C15 H15B . 0.97(2) no
C16 C17 . 1.518(3) no
C16 H16A . 0.98(2) no
C16 H16B . 0.95(3) no
C17 C18 . 1.520(3) no
C17 H17A . 0.95(3) no
C17 H17B . 0.98(3) no
C18 C19 . 1.520(3) no
C18 H18A . 1.02(3) no
C18 H18B . 1.01(3) no
C19 H19A . 0.95(2) no
C19 H19B . 1.03(3) no
