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#$Date: 2016-03-22 11:23:37 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178897 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/26/4112686.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_4112686
loop_
_publ_author_name
'Xuyang He'
'Bruce C. Noll'
'Alicia Beatty'
'Robert E. Mulvey'
'Kenneth W. Henderson'
_publ_contact_author_address
; 
 Department of Chemistry and Biochemistry
 University of Notre Dame
 Notre Dame, IN 46556
;
_publ_contact_author_email       Kenneth.W.Henderson.43@nd.edu
_publ_contact_author_fax         574.631.6652
_publ_contact_author_name        'Professor Kenneth W. Henderson'
_publ_contact_author_phone       574.631.8025
_publ_section_title
;
 Ketone Deprotonation Mediated by Mono- and Heterobimetallic Alkali and
 Alkaline Earth Metal Amide Bases: Structural Characterization of
 Potassium, Calcium, and Mixed Potassium-Calcium Enolates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7444
_journal_page_last               7445
_journal_paper_doi               10.1021/ja048750m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C42 H82 Ca2 N2 O4 Si4'
_chemical_formula_sum            'C42 H82 Ca2 N2 O4 Si4'
_chemical_formula_weight         871.62
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.044(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2784(10)
_cell_length_b                   14.8498(12)
_cell_length_c                   14.4883(12)
_cell_measurement_reflns_used    9215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.568
_cell_measurement_theta_min      2.410
_cell_volume                     2583.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'ω scans'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16910
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9176
_exptl_absorpt_correction_T_min  0.8174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H., Acta Cryst. (1995) A51. 33-8'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+6.3603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1522
_reflns_number_gt                3746
_reflns_number_total             4544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048750msi20040304_085026.cif
_cod_data_source_block           bcn06
_cod_database_code               4112686
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.50349(8) 0.08743(5) 0.41533(6) 0.0451(3) Uani 1 1 d . . .
N1 N 0.6389(3) 0.1317(2) 0.3369(2) 0.0391(8) Uani 1 1 d . A .
O1 O 0.5615(3) 0.05437(18) 0.57125(19) 0.0460(7) Uani 1 1 d . . .
Si1 Si 0.58626(9) 0.19298(6) 0.23901(7) 0.0313(3) Uani 1 1 d . . .
Si2 Si 0.78098(15) 0.10911(11) 0.37687(11) 0.0385(4) Uani 0.85 1 d P A 1
C19 C 0.8609(5) 0.0994(5) 0.2794(4) 0.0580(18) Uani 0.85 1 d P A 1
H19B H 0.9383 0.0828 0.3063 0.087 Uiso 0.85 1 calc PR A 1
H19C H 0.8594 0.1574 0.2468 0.087 Uiso 0.85 1 calc PR A 1
H19A H 0.8267 0.0531 0.2344 0.087 Uiso 0.85 1 calc PR A 1
C20 C 0.8581(5) 0.1943(5) 0.4613(4) 0.0561(17) Uani 0.85 1 d P A 1
H20A H 0.8582 0.2523 0.4290 0.084 Uiso 0.85 1 calc PR A 1
H20B H 0.9350 0.1741 0.4841 0.084 Uiso 0.85 1 calc PR A 1
H20C H 0.8214 0.2011 0.5148 0.084 Uiso 0.85 1 calc PR A 1
C21 C 0.7847(7) -0.0094(4) 0.4353(5) 0.068(2) Uani 0.85 1 d P A 1
H21A H 0.7382 -0.0089 0.4827 0.103 Uiso 0.85 1 calc PR A 1
H21B H 0.8615 -0.0243 0.4658 0.103 Uiso 0.85 1 calc PR A 1
H21C H 0.7563 -0.0545 0.3869 0.103 Uiso 0.85 1 calc PR A 1
Si2' Si 0.7398(5) 0.0933(4) 0.3540(5) 0.0066(15) Uiso 0.15 1 d P A 2
C19' C 0.823(2) 0.0790(17) 0.258(2) 0.017(6) Uiso 0.15 1 d P A 2
C20' C 0.8250(17) 0.1730(12) 0.4375(14) 0.001(4) Uiso 0.15 1 d P A 2
C21' C 0.820(2) 0.0194(18) 0.432(2) 0.023(6) Uiso 0.15 1 d P A 2
C1 C 0.6225(4) 0.1077(3) 0.6379(3) 0.0437(10) Uani 1 1 d . . .
C2 C 0.6506(4) 0.1922(3) 0.6219(4) 0.0606(13) Uani 1 1 d . B .
H2A H 0.6275 0.2179 0.5609 0.073 Uiso 1 1 calc R . .
H2B H 0.6938 0.2267 0.6716 0.073 Uiso 1 1 calc R . .
C3 C 0.6572(3) 0.0656(2) 0.7342(3) 0.0356(9) Uani 1 1 d . B .
C4 C 0.7628(3) 0.0267(2) 0.7623(3) 0.0417(10) Uani 1 1 d . . .
C5 C 0.7915(4) -0.0142(2) 0.8495(3) 0.0455(10) Uani 1 1 d . B .
H5 H 0.8622 -0.0424 0.8671 0.055 Uiso 1 1 calc R . .
C6 C 0.7200(4) -0.0154(2) 0.9123(3) 0.0432(10) Uani 1 1 d . . .
C7 C 0.6169(3) 0.0258(2) 0.8845(3) 0.0375(9) Uani 1 1 d . B .
H7 H 0.5679 0.0271 0.9272 0.045 Uiso 1 1 calc R . .
C8 C 0.5828(3) 0.0651(2) 0.7961(3) 0.0353(9) Uani 1 1 d . . .
C9 C 0.8468(4) 0.0304(3) 0.6988(4) 0.0606(14) Uani 1 1 d . B .
H9A H 0.8745 0.0922 0.6970 0.091 Uiso 1 1 calc R . .
H9B H 0.8109 0.0115 0.6349 0.091 Uiso 1 1 calc R . .
H9C H 0.9092 -0.0100 0.7236 0.091 Uiso 1 1 calc R . .
C10 C 0.7542(4) -0.0606(3) 1.0065(3) 0.0592(13) Uani 1 1 d . B .
H10A H 0.7577 -0.1259 0.9975 0.089 Uiso 1 1 calc R . .
H10B H 0.6996 -0.0471 1.0452 0.089 Uiso 1 1 calc R . .
H10C H 0.8276 -0.0384 1.0383 0.089 Uiso 1 1 calc R . .
C11 C 0.4686(4) 0.1067(3) 0.7686(3) 0.0459(11) Uani 1 1 d . B .
H11A H 0.4154 0.0612 0.7378 0.069 Uiso 1 1 calc R . .
H11B H 0.4706 0.1567 0.7249 0.069 Uiso 1 1 calc R . .
H11C H 0.4455 0.1291 0.8252 0.069 Uiso 1 1 calc R . .
O2 O 0.3388(4) 0.1775(3) 0.4300(3) 0.0473(15) Uani 0.682(6) 1 d P B 1
C12 C 0.3569(7) 0.2259(5) 0.5183(5) 0.0486(19) Uani 0.682(6) 1 d P B 1
H12A H 0.4158 0.1951 0.5647 0.058 Uiso 0.682(6) 1 calc PR B 1
H12B H 0.2876 0.2248 0.5431 0.058 Uiso 0.682(6) 1 calc PR B 1
C13 C 0.3915(8) 0.3239(4) 0.5077(6) 0.063(2) Uani 0.682(6) 1 d P B 1
H13C H 0.3312 0.3558 0.4654 0.095 Uiso 0.682(6) 1 calc PR B 1
H13A H 0.4587 0.3253 0.4812 0.095 Uiso 0.682(6) 1 calc PR B 1
H13B H 0.4069 0.3531 0.5697 0.095 Uiso 0.682(6) 1 calc PR B 1
C14 C 0.2407(6) 0.2071(4) 0.3616(4) 0.0455(17) Uani 0.682(6) 1 d P B 1
H14A H 0.2312 0.1676 0.3054 0.055 Uiso 0.682(6) 1 calc PR B 1
H14B H 0.2540 0.2690 0.3411 0.055 Uiso 0.682(6) 1 calc PR B 1
C15 C 0.1357(7) 0.2065(4) 0.3971(6) 0.057(2) Uani 0.682(6) 1 d P B 1
H15A H 0.1293 0.1493 0.4294 0.086 Uiso 0.682(6) 1 calc PR B 1
H15B H 0.0722 0.2132 0.3439 0.086 Uiso 0.682(6) 1 calc PR B 1
H15C H 0.1363 0.2564 0.4413 0.086 Uiso 0.682(6) 1 calc PR B 1
O2' O 0.4157(7) 0.2121(5) 0.4652(5) 0.024(2) Uiso 0.318(6) 1 d P B 2
C12' C 0.4347(8) 0.3078(7) 0.4552(7) 0.023(2) Uiso 0.318(6) 1 d P B 2
C13' C 0.4481(12) 0.3573(10) 0.5496(10) 0.041(3) Uiso 0.318(6) 1 d P B 2
C14' C 0.3124(11) 0.1888(10) 0.4935(10) 0.034(3) Uiso 0.318(6) 1 d P B 2
C15' C 0.2105(15) 0.2167(10) 0.4254(12) 0.050(4) Uiso 0.318(6) 1 d P B 2
C16 C 0.4321(3) 0.2031(3) 0.2278(3) 0.0445(10) Uani 1 1 d . B .
H16A H 0.3998 0.1431 0.2305 0.067 Uiso 1 1 calc R . .
H16B H 0.3992 0.2316 0.1673 0.067 Uiso 1 1 calc R . .
H16C H 0.4165 0.2401 0.2796 0.067 Uiso 1 1 calc R . .
C17 C 0.6413(4) 0.3108(3) 0.2422(3) 0.0470(11) Uani 1 1 d . B .
H17A H 0.6245 0.3425 0.2969 0.071 Uiso 1 1 calc R . .
H17B H 0.6060 0.3424 0.1843 0.071 Uiso 1 1 calc R . .
H17C H 0.7221 0.3092 0.2471 0.071 Uiso 1 1 calc R . .
C18 C 0.6054(4) 0.1429(3) 0.1242(3) 0.0432(10) Uani 1 1 d . B .
H18A H 0.6818 0.1536 0.1167 0.065 Uiso 1 1 calc R . .
H18B H 0.5530 0.1710 0.0718 0.065 Uiso 1 1 calc R . .
H18C H 0.5914 0.0779 0.1244 0.065 Uiso 1 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'
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'
Ca Ca 0.2262 0.3064 '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'
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
O1 Ca1 O1 76.01(12) 3_656 .
O1 Ca1 N1 127.60(10) 3_656 .
O1 Ca1 N1 116.35(12) . .
O1 Ca1 O2' 121.0(2) 3_656 .
O1 Ca1 O2' 86.16(19) . .
N1 Ca1 O2' 110.8(2) . .
O1 Ca1 O2 100.72(13) 3_656 .
O1 Ca1 O2 97.11(12) . .
N1 Ca1 O2 125.28(12) . .
O2' Ca1 O2 26.32(19) . .
O1 Ca1 Ca1 38.02(7) 3_656 3_656
O1 Ca1 Ca1 37.99(7) . 3_656
N1 Ca1 Ca1 131.97(9) . 3_656
O2' Ca1 Ca1 106.52(17) . 3_656
O2 Ca1 Ca1 101.33(9) . 3_656
Si2' N1 Si1 124.1(3) . .
Si1 N1 Si2 123.99(18) . .
Si2' N1 Ca1 121.6(3) . .
Si1 N1 Ca1 112.23(17) . .
Si2 N1 Ca1 123.71(16) . .
C1 O1 Ca1 129.4(2) . 3_656
C1 O1 Ca1 126.6(2) . .
Ca1 O1 Ca1 103.99(12) 3_656 .
N1 Si1 C16 108.56(17) . .
N1 Si1 C17 114.11(19) . .
C16 Si1 C17 106.3(2) . .
N1 Si1 C18 115.51(17) . .
C16 Si1 C18 105.41(19) . .
C17 Si1 C18 106.28(18) . .
N1 Si2 C20 114.8(2) . .
N1 Si2 C19 113.9(2) . .
C20 Si2 C19 105.6(3) . .
N1 Si2 C21 104.3(3) . .
C20 Si2 C21 111.3(3) . .
C19 Si2 C21 106.7(3) . .
N1 Si2' C21' 140.4(10) . .
N1 Si2' C20' 102.9(7) . .
C21' Si2' C20' 79.2(11) . .
N1 Si2' C19' 121.9(10) . .
C21' Si2' C19' 95.1(13) . .
C20' Si2' C19' 103.5(10) . .
C2 C1 O1 123.6(4) . .
C2 C1 C3 121.1(4) . .
O1 C1 C3 115.3(3) . .
C1 C2 H2A 120.0 . .
C1 C2 H2B 120.0 . .
H2A C2 H2B 120.0 . .
C4 C3 C8 119.9(4) . .
C4 C3 C1 120.4(3) . .
C8 C3 C1 119.8(4) . .
C5 C4 C3 119.4(4) . .
C5 C4 C9 119.7(4) . .
C3 C4 C9 120.9(4) . .
C4 C5 C6 122.0(4) . .
C4 C5 H5 119.0 . .
C6 C5 H5 119.0 . .
C7 C6 C5 117.7(4) . .
C7 C6 C10 121.8(4) . .
C5 C6 C10 120.4(4) . .
C6 C7 C8 122.3(3) . .
C6 C7 H7 118.9 . .
C8 C7 H7 118.9 . .
C7 C8 C3 118.6(4) . .
C7 C8 C11 120.0(3) . .
C3 C8 C11 121.4(4) . .
C4 C9 H9A 109.5 . .
C4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C10 H10A 109.5 . .
C6 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C6 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C12 O2 C14 113.9(4) . .
C12 O2 Ca1 111.6(4) . .
C14 O2 Ca1 132.8(3) . .
O2 C12 C13 112.2(5) . .
O2 C12 H12A 109.2 . .
C13 C12 H12A 109.2 . .
O2 C12 H12B 109.2 . .
C13 C12 H12B 109.2 . .
H12A C12 H12B 107.9 . .
O2 C14 C15 114.6(5) . .
O2 C14 H14A 108.6 . .
C15 C14 H14A 108.6 . .
O2 C14 H14B 108.6 . .
C15 C14 H14B 108.6 . .
H14A C14 H14B 107.6 . .
C12' O2' C14' 115.4(8) . .
C12' O2' Ca1 130.7(6) . .
C14' O2' Ca1 112.7(7) . .
O2' C12' C13' 111.7(9) . .
O2' C14' C15' 114.3(12) . .
Si1 C16 H16A 109.5 . .
Si1 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
Si1 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
Si1 C17 H17A 109.5 . .
Si1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
Si1 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
Si1 C18 H18A 109.5 . .
Si1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
Si1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.275(3) 3_656
Ca1 O1 2.276(3) .
Ca1 N1 2.297(3) .
Ca1 O2' 2.331(7) .
Ca1 O2 2.471(4) .
Ca1 Ca1 3.5857(14) 3_656
N1 Si2' 1.339(7) .
N1 Si1 1.695(3) .
N1 Si2 1.752(4) .
O1 C1 1.348(5) .
O1 Ca1 2.275(3) 3_656
Si1 C16 1.872(4) .
Si1 C17 1.873(4) .
Si1 C18 1.881(4) .
Si2 C20 1.874(7) .
Si2 C19 1.886(5) .
Si2 C21 1.949(6) .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C19 H19A 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
Si2' C21' 1.72(3) .
Si2' C20' 1.85(2) .
Si2' C19' 1.91(3) .
C1 C2 1.335(6) .
C1 C3 1.508(6) .
C2 H2A 0.9500 .
C2 H2B 0.9500 .
C3 C4 1.400(6) .
C3 C8 1.407(5) .
C4 C5 1.379(6) .
C4 C9 1.519(5) .
C5 C6 1.391(6) .
C5 H5 0.9500 .
C6 C7 1.388(6) .
C6 C10 1.499(6) .
C7 C8 1.390(6) .
C7 H7 0.9500 .
C8 C11 1.508(6) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
O2 C12 1.443(9) .
O2 C14 1.459(8) .
C12 C13 1.533(10) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 H13C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C14 C15 1.484(9) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
O2' C12' 1.453(12) .
O2' C14' 1.453(16) .
C12' C13' 1.531(17) .
C14' C15' 1.48(2) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
