#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:25:42 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179843 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/39/7013962.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_7013962
loop_
_publ_author_name
'Avent, Anthony G.'
'Caro, Catherine F.'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Li, Zhengning'
'Wei, Xue-Hong'
_publ_section_title
;
 Synthetic and structural experiments on yttrium, cerium and magnesium
 trimethylsilylmethyls and their reaction products with nitriles; with
 a note on two cerium beta-diketiminates.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1567
_journal_page_last               1577
_journal_paper_doi               10.1039/b316695n
_journal_year                    2004
_chemical_formula_sum            'C22 H58 Br2 Mg2 O2 Si4'
_chemical_formula_weight         675.48
_chemical_name_systematic
;
?
;
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.184(2)
_cell_length_b                   9.244(2)
_cell_length_c                   25.873(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3683.2(11)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6694
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.381
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_obs          0.0738
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1274P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2054
_refine_ls_wR_factor_obs         0.1761
_reflns_number_observed          4335
_reflns_number_total             6462
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b316695n.txt
_cod_data_source_block           (D)-aug1297
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Br1 Br 0.40207(5) 0.40222(8) 0.22988(3) 0.0365(2) Uani 1 d . .
Br2 Br 0.57616(5) 0.67110(8) 0.26069(3) 0.0392(2) Uani 1 d . .
Si1 Si 0.37127(13) 0.4519(2) 0.05902(8) 0.0297(4) Uani 1 d . .
Si2 Si 0.45878(14) 0.7620(2) 0.08715(8) 0.0334(5) Uani 1 d . .
Si3 Si 0.4994(2) 0.2847(2) 0.40056(8) 0.0410(5) Uani 1 d . .
Si4 Si 0.63346(13) 0.5489(2) 0.42775(8) 0.0391(5) Uani 1 d . .
Mg1 Mg 0.50543(15) 0.5023(2) 0.17982(9) 0.0295(5) Uani 1 d . .
Mg2 Mg 0.47878(15) 0.5599(2) 0.31307(9) 0.0293(5) Uani 1 d . .
O1 O 0.5978(3) 0.3475(5) 0.1910(2) 0.0428(13) Uani 1 d . .
O2 O 0.3933(3) 0.7216(5) 0.3095(2) 0.0391(12) Uani 1 d . .
C1 C 0.4639(4) 0.5650(7) 0.0972(3) 0.0284(15) Uani 1 d . .
H1 H 0.5124 0.5337 0.0834 0.034 Uiso 1 calc R .
C2 C 0.3518(6) 0.4516(9) -0.0162(3) 0.048(2) Uani 1 d . .
H2A H 0.3019 0.3897 -0.0337 0.073 Uiso 1 calc R .
H2B H 0.4034 0.4146 -0.0240 0.073 Uiso 1 calc R .
H2C H 0.3399 0.5505 -0.0302 0.073 Uiso 1 calc R .
C3 C 0.3915(5) 0.2580(8) 0.0807(3) 0.042(2) Uani 1 d . .
H3A H 0.3421 0.1988 0.0602 0.064 Uiso 1 calc R .
H3B H 0.3988 0.2501 0.1196 0.064 Uiso 1 calc R .
H3C H 0.4443 0.2240 0.0735 0.064 Uiso 1 calc R .
C4 C 0.2665(5) 0.5114(9) 0.0700(3) 0.045(2) Uani 1 d . .
H4A H 0.2191 0.4489 0.0491 0.067 Uiso 1 calc R .
H4B H 0.2541 0.6117 0.0579 0.067 Uiso 1 calc R .
H4C H 0.2719 0.5045 0.1087 0.067 Uiso 1 calc R .
C5 C 0.5707(5) 0.8394(9) 0.1128(3) 0.051(2) Uani 1 d . .
H5A H 0.5681 0.9445 0.1074 0.077 Uiso 1 calc R .
H5B H 0.6072 0.7966 0.0928 0.077 Uiso 1 calc R .
H5C H 0.5956 0.8178 0.1516 0.077 Uiso 1 calc R .
C6 C 0.3919(6) 0.8497(8) 0.1253(3) 0.047(2) Uani 1 d . .
H6A H 0.3904 0.9544 0.1191 0.071 Uiso 1 calc R .
H6B H 0.4174 0.8299 0.1642 0.071 Uiso 1 calc R .
H6C H 0.3327 0.8109 0.1127 0.071 Uiso 1 calc R .
C7 C 0.4156(6) 0.8206(9) 0.0143(3) 0.054(2) Uani 1 d . .
H7A H 0.4149 0.9265 0.0124 0.081 Uiso 1 calc R .
H7B H 0.3565 0.7835 -0.0015 0.081 Uiso 1 calc R .
H7C H 0.4530 0.7823 -0.0060 0.081 Uiso 1 calc R .
C8 C 0.6263(6) 0.2578(9) 0.2396(3) 0.058(2) Uani 1 d . .
H8A H 0.6093 0.3040 0.2693 0.069 Uiso 1 calc R .
H8B H 0.6904 0.2494 0.2514 0.069 Uiso 1 calc R .
C9 C 0.5862(9) 0.1089(10) 0.2285(4) 0.087(4) Uani 1 d . .
H9A H 0.6060 0.0501 0.2615 0.130 Uiso 1 calc R .
H9B H 0.6039 0.0627 0.1994 0.130 Uiso 1 calc R .
H9C H 0.5228 0.1173 0.2173 0.130 Uiso 1 calc R .
C10 C 0.6498(6) 0.3301(11) 0.1549(4) 0.068(3) Uani 1 d . .
H10A H 0.6123 0.3410 0.1169 0.081 Uiso 1 calc R .
H10B H 0.6747 0.2314 0.1592 0.081 Uiso 1 calc R .
C11 C 0.7201(7) 0.4363(14) 0.1662(4) 0.089(4) Uani 1 d . .
H11A H 0.7539 0.4215 0.1410 0.133 Uiso 1 calc R .
H11B H 0.7579 0.4245 0.2036 0.133 Uiso 1 calc R .
H11C H 0.6955 0.5341 0.1614 0.133 Uiso 1 calc R .
C12 C 0.5248(5) 0.4758(7) 0.3933(2) 0.031(2) Uani 1 d . .
H12 H 0.4877 0.5270 0.4121 0.038 Uiso 1 calc R .
C13 C 0.3807(6) 0.2526(9) 0.3698(3) 0.055(2) Uani 1 d . .
H13A H 0.3678 0.1505 0.3738 0.082 Uiso 1 calc R .
H13B H 0.3634 0.2776 0.3311 0.082 Uiso 1 calc R .
H13C H 0.3486 0.3130 0.3881 0.082 Uiso 1 calc R .
C14 C 0.5562(7) 0.1628(9) 0.3656(4) 0.073(3) Uani 1 d . .
H14A H 0.5410 0.0621 0.3704 0.109 Uiso 1 calc R .
H14B H 0.6191 0.1757 0.3812 0.109 Uiso 1 calc R .
H14C H 0.5385 0.1861 0.3268 0.109 Uiso 1 calc R .
C15 C 0.5271(7) 0.2213(10) 0.4732(3) 0.076(3) Uani 1 d . .
H15A H 0.5118 0.1189 0.4738 0.114 Uiso 1 calc R .
H15B H 0.4945 0.2784 0.4922 0.114 Uiso 1 calc R .
H15C H 0.5895 0.2336 0.4912 0.114 Uiso 1 calc R .
C16 C 0.7167(5) 0.4764(11) 0.3975(4) 0.061(3) Uani 1 d . .
H16A H 0.7736 0.5175 0.4168 0.092 Uiso 1 calc R .
H16B H 0.7006 0.5031 0.3590 0.092 Uiso 1 calc R .
H16C H 0.7192 0.3708 0.4010 0.092 Uiso 1 calc R .
C17 C 0.6740(6) 0.5114(11) 0.5023(3) 0.071(3) Uani 1 d . .
H17A H 0.7319 0.5536 0.5177 0.107 Uiso 1 calc R .
H17B H 0.6771 0.4066 0.5084 0.107 Uiso 1 calc R .
H17C H 0.6342 0.5543 0.5200 0.107 Uiso 1 calc R .
C18 C 0.6330(5) 0.7503(9) 0.4214(3) 0.051(2) Uani 1 d . .
H18A H 0.6913 0.7879 0.4399 0.077 Uiso 1 calc R .
H18B H 0.5915 0.7916 0.4381 0.077 Uiso 1 calc R .
H18C H 0.6161 0.7771 0.3829 0.077 Uiso 1 calc R .
C19 C 0.3679(6) 0.7645(9) 0.3580(3) 0.052(2) Uani 1 d . .
H19A H 0.4187 0.7544 0.3910 0.063 Uiso 1 calc R .
H19B H 0.3502 0.8675 0.3547 0.063 Uiso 1 calc R .
C20 C 0.2968(6) 0.6769(10) 0.3641(4) 0.064(3) Uani 1 d . .
H20A H 0.2822 0.7084 0.3964 0.096 Uiso 1 calc R .
H20B H 0.3145 0.5750 0.3682 0.096 Uiso 1 calc R .
H20C H 0.2460 0.6881 0.3319 0.096 Uiso 1 calc R .
C21 C 0.3395(6) 0.7856(9) 0.2602(3) 0.058(2) Uani 1 d . .
H21A H 0.2778 0.7766 0.2586 0.070 Uiso 1 calc R .
H21B H 0.3474 0.7325 0.2288 0.070 Uiso 1 calc R .
C22 C 0.3610(9) 0.9433(10) 0.2561(4) 0.088(4) Uani 1 d . .
H22A H 0.3231 0.9833 0.2219 0.133 Uiso 1 calc R .
H22B H 0.4217 0.9524 0.2569 0.133 Uiso 1 calc R .
H22C H 0.3522 0.9965 0.2867 0.133 Uiso 1 calc R .
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mg2 Br1 Mg1 89.79(7) . . ?
Mg1 Br2 Mg2 89.69(7) . . ?
C1 Si1 C2 114.0(3) . . ?
C1 Si1 C3 110.0(3) . . ?
C2 Si1 C3 105.5(4) . . ?
C1 Si1 C4 112.0(3) . . ?
C2 Si1 C4 106.6(4) . . ?
C3 Si1 C4 108.4(4) . . ?
C1 Si2 C6 111.4(3) . . ?
C1 Si2 C5 109.4(4) . . ?
C6 Si2 C5 107.7(4) . . ?
C1 Si2 C7 114.5(3) . . ?
C6 Si2 C7 108.0(4) . . ?
C5 Si2 C7 105.4(4) . . ?
C12 Si3 C14 112.0(4) . . ?
C12 Si3 C13 110.1(4) . . ?
C14 Si3 C13 107.2(4) . . ?
C12 Si3 C15 114.1(4) . . ?
C14 Si3 C15 107.1(5) . . ?
C13 Si3 C15 106.0(4) . . ?
C12 Si4 C18 110.3(3) . . ?
C12 Si4 C17 114.3(4) . . ?
C18 Si4 C17 105.4(4) . . ?
C12 Si4 C16 111.6(4) . . ?
C18 Si4 C16 107.6(4) . . ?
C17 Si4 C16 107.2(4) . . ?
O1 Mg1 C1 109.2(2) . . ?
O1 Mg1 Br2 100.8(2) . . ?
C1 Mg1 Br2 125.3(2) . . ?
O1 Mg1 Br1 103.8(2) . . ?
C1 Mg1 Br1 123.5(2) . . ?
Br2 Mg1 Br1 90.24(7) . . ?
O2 Mg2 C12 110.2(2) . . ?
O2 Mg2 Br1 103.4(2) . . ?
C12 Mg2 Br1 122.9(2) . . ?
O2 Mg2 Br2 101.6(2) . . ?
C12 Mg2 Br2 124.7(2) . . ?
Br1 Mg2 Br2 90.11(7) . . ?
C10 O1 C8 113.6(6) . . ?
C10 O1 Mg1 122.5(5) . . ?
C8 O1 Mg1 123.3(5) . . ?
C21 O2 C19 113.1(6) . . ?
C21 O2 Mg2 124.5(4) . . ?
C19 O2 Mg2 121.4(4) . . ?
Si2 C1 Si1 119.4(4) . . ?
Si2 C1 Mg1 113.7(3) . . ?
Si1 C1 Mg1 109.8(3) . . ?
O1 C8 C9 110.5(7) . . ?
O1 C10 C11 111.6(8) . . ?
Si3 C12 Si4 121.0(4) . . ?
Si3 C12 Mg2 115.4(3) . . ?
Si4 C12 Mg2 109.6(3) . . ?
C20 C19 O2 112.0(7) . . ?
O2 C21 C22 111.8(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Mg2 2.580(2) . ?
Br1 Mg1 2.582(2) . ?
Br2 Mg1 2.579(2) . ?
Br2 Mg2 2.587(2) . ?
Si1 C1 1.846(7) . ?
Si1 C2 1.873(7) . ?
Si1 C3 1.876(8) . ?
Si1 C4 1.884(7) . ?
Si2 C1 1.838(7) . ?
Si2 C6 1.860(7) . ?
Si2 C5 1.870(8) . ?
Si2 C7 1.877(8) . ?
Si3 C12 1.837(7) . ?
Si3 C14 1.856(9) . ?
Si3 C13 1.862(9) . ?
Si3 C15 1.885(8) . ?
Si4 C12 1.838(7) . ?
Si4 C18 1.869(8) . ?
Si4 C17 1.870(8) . ?
Si4 C16 1.876(8) . ?
Mg1 O1 2.024(5) . ?
Mg1 C1 2.114(7) . ?
Mg2 O2 2.020(5) . ?
Mg2 C12 2.125(6) . ?
O1 C10 1.444(9) . ?
O1 C8 1.458(9) . ?
O2 C21 1.432(9) . ?
O2 C19 1.491(8) . ?
C8 C9 1.512(13) . ?
C10 C11 1.463(14) . ?
C19 C20 1.454(12) . ?
C21 C22 1.510(13) . ?
