#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308297.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_4308297
loop_
_publ_author_name
'Martin Gärtner'
'Reinald Fischer'
'Jens Langer'
'Helmar Görls'
'Dirk Walther'
'Matthias Westerhausen'
_publ_contact_author
;
      Matthias Westerhausen
      Institut für anorganische und analytische Chemie
      Friedrich-Schiller-Universität Jena
      August-Bebel-Str. 2
      07743 Jena
      Germany
;
_publ_contact_author_email       m.we@uni-jena.de
_publ_contact_author_fax         '03641 948 102'
_publ_contact_author_phone       '03641 948 110'
_publ_section_title
;
Syntheses and Structures of Alkaline Earth Metal Bis(diphenylamides)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5118
_journal_page_last               5124
_journal_paper_doi               10.1021/ic700459d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C32 H40 Ca N2 O4'
_chemical_formula_weight         556.74
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 129.216(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.9375(8)
_cell_length_b                   17.2162(5)
_cell_length_c                   18.4757(6)
_cell_measurement_temperature    183(2)
_cell_volume                     6145.6(4)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20544
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0564P)²+0.8388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                4811
_reflns_number_total             7029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700459d-file001_3.cif
_cod_data_source_block           FO3030
_cod_original_cell_volume        6145.6(3)
_cod_database_code               4308297
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_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
CaA Ca 0.5000 0.50215(3) 0.7500 0.02577(12) Uani 1 2 d S . .
O1A O 0.59310(6) 0.59909(7) 0.84776(9) 0.0356(3) Uani 1 1 d . . .
O2A O 0.49358(7) 0.57070(7) 0.86032(9) 0.0357(3) Uani 1 1 d . . .
N1A N 0.40716(8) 0.41227(9) 0.66895(10) 0.0321(3) Uani 1 1 d . . .
C1A C 0.39268(10) 0.38261(10) 0.72554(13) 0.0322(4) Uani 1 1 d . . .
C2A C 0.32519(10) 0.37813(11) 0.69707(14) 0.0376(4) Uani 1 1 d . . .
H2AA H 0.2867 0.3929 0.6353 0.045 Uiso 1 1 calc R . .
C3A C 0.31427(12) 0.35255(12) 0.75787(16) 0.0467(5) Uani 1 1 d . . .
H3AA H 0.2684 0.3494 0.7371 0.056 Uiso 1 1 calc R . .
C4A C 0.36961(13) 0.33150(13) 0.84892(16) 0.0511(6) Uani 1 1 d . . .
H4AA H 0.3619 0.3137 0.8903 0.061 Uiso 1 1 calc R . .
C5A C 0.43595(12) 0.33678(11) 0.87837(14) 0.0447(5) Uani 1 1 d . . .
H5AA H 0.4741 0.3230 0.9407 0.054 Uiso 1 1 calc R . .
C6A C 0.44752(10) 0.36195(10) 0.81792(13) 0.0354(4) Uani 1 1 d . . .
H6AA H 0.4936 0.3652 0.8397 0.042 Uiso 1 1 calc R . .
C7A C 0.36726(9) 0.38959(10) 0.57704(13) 0.0311(4) Uani 1 1 d . . .
C8A C 0.36766(9) 0.43537(11) 0.51367(13) 0.0355(4) Uani 1 1 d . . .
H8AA H 0.3934 0.4824 0.5350 0.043 Uiso 1 1 calc R . .
C9A C 0.33153(10) 0.41328(13) 0.42146(14) 0.0414(5) Uani 1 1 d . . .
H9AA H 0.3325 0.4457 0.3807 0.050 Uiso 1 1 calc R . .
C10A C 0.29399(10) 0.34486(13) 0.38744(14) 0.0448(5) Uani 1 1 d . . .
H10A H 0.2689 0.3302 0.3240 0.054 Uiso 1 1 calc R . .
C11A C 0.29412(10) 0.29826(12) 0.44907(15) 0.0434(5) Uani 1 1 d . . .
H11A H 0.2694 0.2506 0.4274 0.052 Uiso 1 1 calc R . .
C12A C 0.32931(10) 0.31973(11) 0.54093(14) 0.0369(4) Uani 1 1 d . . .
H12A H 0.3279 0.2866 0.5809 0.044 Uiso 1 1 calc R . .
C13A C 0.66228(10) 0.58788(13) 0.88077(15) 0.0444(5) Uani 1 1 d . . .
H13A H 0.6812 0.6377 0.8804 0.067 Uiso 1 1 calc R . .
H13B H 0.6618 0.5511 0.8399 0.067 Uiso 1 1 calc R . .
H13C H 0.6912 0.5672 0.9446 0.067 Uiso 1 1 calc R . .
C14A C 0.59133(11) 0.64610(12) 0.90942(15) 0.0455(5) Uani 1 1 d . . .
H14A H 0.6081 0.6991 0.9123 0.055 Uiso 1 1 calc R . .
H14B H 0.6217 0.6237 0.9731 0.055 Uiso 1 1 calc R . .
C15A C 0.51811(11) 0.64958(11) 0.87379(15) 0.0414(5) Uani 1 1 d . . .
H15A H 0.5162 0.6766 0.9195 0.050 Uiso 1 1 calc R . .
H15B H 0.4888 0.6784 0.8140 0.050 Uiso 1 1 calc R . .
C16A C 0.44110(11) 0.56349(12) 0.86987(16) 0.0459(5) Uani 1 1 d . . .
H16A H 0.4615 0.5724 0.9351 0.069 Uiso 1 1 calc R . .
H16B H 0.4212 0.5112 0.8511 0.069 Uiso 1 1 calc R . .
H16C H 0.4047 0.6019 0.8300 0.069 Uiso 1 1 calc R . .
CaB Ca 0.0000 0.49096(3) 0.2500 0.02508(12) Uani 1 2 d S . .
O1B O -0.00836(7) 0.38075(7) 0.32534(9) 0.0378(3) Uani 1 1 d . . .
O2B O -0.11798(6) 0.45456(8) 0.17405(9) 0.0381(3) Uani 1 1 d . . .
N1B N 0.01220(8) 0.57629(8) 0.36102(10) 0.0318(3) Uani 1 1 d . . .
C1B C -0.03706(9) 0.63165(10) 0.33438(12) 0.0292(4) Uani 1 1 d . . .
C2B C -0.04668(10) 0.66602(10) 0.39516(13) 0.0336(4) Uani 1 1 d . . .
H2BA H -0.0146 0.6551 0.4602 0.040 Uiso 1 1 calc R . .
C3B C -0.10189(10) 0.71509(11) 0.36177(14) 0.0406(5) Uani 1 1 d . . .
H3BA H -0.1068 0.7373 0.4044 0.049 Uiso 1 1 calc R . .
C4B C -0.14981(11) 0.73246(12) 0.26821(15) 0.0451(5) Uani 1 1 d . . .
H4BA H -0.1881 0.7653 0.2459 0.054 Uiso 1 1 calc R . .
C5B C -0.14105(11) 0.70088(12) 0.20697(15) 0.0448(5) Uani 1 1 d . . .
H5BA H -0.1735 0.7126 0.1422 0.054 Uiso 1 1 calc R . .
C6B C -0.08563(10) 0.65265(11) 0.23950(13) 0.0391(4) Uani 1 1 d . . .
H6BA H -0.0801 0.6330 0.1965 0.047 Uiso 1 1 calc R . .
C7B C 0.07069(9) 0.57206(10) 0.45548(12) 0.0306(4) Uani 1 1 d . . .
C8B C 0.08984(11) 0.50194(11) 0.50399(14) 0.0428(5) Uani 1 1 d . . .
H8BA H 0.0597 0.4585 0.4749 0.051 Uiso 1 1 calc R . .
C9B C 0.15221(13) 0.49440(14) 0.59410(15) 0.0545(6) Uani 1 1 d . . .
H9BA H 0.1644 0.4456 0.6249 0.065 Uiso 1 1 calc R . .
C10B C 0.19610(11) 0.55591(15) 0.63904(15) 0.0536(6) Uani 1 1 d . . .
H10B H 0.2389 0.5502 0.7003 0.064 Uiso 1 1 calc R . .
C11B C 0.17731(12) 0.62605(15) 0.59402(17) 0.0564(6) Uani 1 1 d . . .
H11B H 0.2071 0.6696 0.6249 0.068 Uiso 1 1 calc R . .
C12B C 0.11541(11) 0.63448(12) 0.50392(15) 0.0471(5) Uani 1 1 d . . .
H12B H 0.1033 0.6839 0.4747 0.056 Uiso 1 1 calc R . .
C13B C 0.04070(12) 0.31905(12) 0.37438(15) 0.0504(5) Uani 1 1 d . . .
H13D H 0.0456 0.3053 0.4298 0.076 Uiso 1 1 calc R . .
H13E H 0.0856 0.3359 0.3936 0.076 Uiso 1 1 calc R . .
H13F H 0.0246 0.2737 0.3334 0.076 Uiso 1 1 calc R . .
C14B C -0.07574(11) 0.36139(13) 0.29429(15) 0.0476(5) Uani 1 1 d . . .
H14C H -0.0732 0.3467 0.3482 0.057 Uiso 1 1 calc R . .
H14D H -0.0949 0.3169 0.2505 0.057 Uiso 1 1 calc R . .
C15B C -0.12080(11) 0.43101(13) 0.24656(14) 0.0458(5) Uani 1 1 d . . .
H15C H -0.1690 0.4183 0.2191 0.055 Uiso 1 1 calc R . .
H15D H -0.1044 0.4737 0.2921 0.055 Uiso 1 1 calc R . .
C16B C -0.18175(10) 0.48812(14) 0.09499(15) 0.0490(5) Uani 1 1 d . . .
H16D H -0.2185 0.4490 0.0657 0.073 Uiso 1 1 calc R . .
H16E H -0.1762 0.5061 0.0497 0.073 Uiso 1 1 calc R . .
H16F H -0.1940 0.5322 0.1156 0.073 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'
N N 0.0061 0.0033 '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'
Ca Ca 0.2262 0.3064 '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
N1A CaA N1A 98.44(8) . 2_656 ?
N1A CaA O2A 109.94(5) . 2_656 ?
N1A CaA O2A 106.81(5) 2_656 2_656 ?
N1A CaA O2A 106.81(5) . . ?
N1A CaA O2A 109.94(5) 2_656 . ?
O2A CaA O2A 122.32(6) 2_656 . ?
N1A CaA O1A 83.59(5) . 2_656 ?
N1A CaA O1A 172.67(5) 2_656 2_656 ?
O2A CaA O1A 65.94(4) 2_656 2_656 ?
O2A CaA O1A 75.97(4) . 2_656 ?
N1A CaA O1A 172.67(5) . . ?
N1A CaA O1A 83.59(5) 2_656 . ?
O2A CaA O1A 75.98(4) 2_656 . ?
O2A CaA O1A 65.94(4) . . ?
O1A CaA O1A 95.29(6) 2_656 . ?
N1A CaA C1A 24.13(5) . . ?
N1A CaA C1A 93.76(5) 2_656 . ?
O2A CaA C1A 133.44(5) 2_656 . ?
O2A CaA C1A 86.44(4) . . ?
O1A CaA C1A 90.91(4) 2_656 . ?
O1A CaA C1A 149.09(4) . . ?
N1A CaA C1A 93.76(5) . 2_656 ?
N1A CaA C1A 24.13(5) 2_656 2_656 ?
O2A CaA C1A 86.45(4) 2_656 2_656 ?
O2A CaA C1A 133.44(5) . 2_656 ?
O1A CaA C1A 149.09(4) 2_656 2_656 ?
O1A CaA C1A 90.91(4) . 2_656 ?
C1A CaA C1A 99.15(7) . 2_656 ?
C14A O1A C13A 112.01(15) . . ?
C14A O1A CaA 118.59(11) . . ?
C13A O1A CaA 122.73(11) . . ?
C16A O2A C15A 112.36(14) . . ?
C16A O2A CaA 127.38(11) . . ?
C15A O2A CaA 110.70(10) . . ?
C7A N1A C1A 119.46(15) . . ?
C7A N1A CaA 128.40(11) . . ?
C1A N1A CaA 112.11(11) . . ?
C6A C1A N1A 119.26(16) . . ?
C6A C1A C2A 117.11(17) . . ?
N1A C1A C2A 123.42(17) . . ?
C6A C1A CaA 84.57(11) . . ?
N1A C1A CaA 43.76(8) . . ?
C2A C1A CaA 141.93(12) . . ?
C3A C2A C1A 120.96(19) . . ?
C2A C3A C4A 120.7(2) . . ?
C5A C4A C3A 119.06(19) . . ?
C4A C5A C6A 120.7(2) . . ?
C5A C6A C1A 121.39(19) . . ?
N1A C7A C12A 124.87(16) . . ?
N1A C7A C8A 119.02(16) . . ?
C12A C7A C8A 115.90(17) . . ?
C9A C8A C7A 121.66(18) . . ?
C8A C9A C10A 121.31(19) . . ?
C9A C10A C11A 117.93(18) . . ?
C12A C11A C10A 121.51(19) . . ?
C11A C12A C7A 121.68(18) . . ?
O1A C14A C15A 108.49(16) . . ?
O2A C15A C14A 107.65(16) . . ?
N1B CaB N1B 103.81(7) . 2 ?
N1B CaB O2B 96.09(5) . . ?
N1B CaB O2B 102.42(5) 2 . ?
N1B CaB O2B 102.42(5) . 2 ?
N1B CaB O2B 96.09(5) 2 2 ?
O2B CaB O2B 149.83(7) . 2 ?
N1B CaB O1B 89.93(5) . . ?
N1B CaB O1B 163.99(5) 2 . ?
O2B CaB O1B 67.43(4) . . ?
O2B CaB O1B 88.78(5) 2 . ?
N1B CaB O1B 163.99(5) . 2 ?
N1B CaB O1B 89.93(5) 2 2 ?
O2B CaB O1B 88.79(5) . 2 ?
O2B CaB O1B 67.43(4) 2 2 ?
O1B CaB O1B 77.85(6) . 2 ?
N1B CaB C15B 79.57(6) . . ?
N1B CaB C15B 125.85(5) 2 . ?
O2B CaB C15B 26.03(5) . . ?
O2B CaB C15B 136.71(5) 2 . ?
O1B CaB C15B 47.94(5) . . ?
O1B CaB C15B 99.18(5) 2 . ?
N1B CaB C15B 125.85(5) . 2 ?
N1B CaB C15B 79.57(6) 2 2 ?
O2B CaB C15B 136.71(5) . 2 ?
O2B CaB C15B 26.03(5) 2 2 ?
O1B CaB C15B 99.18(5) . 2 ?
O1B CaB C15B 47.95(5) 2 2 ?
C15B CaB C15B 141.71(9) . 2 ?
C13B O1B C14B 113.50(15) . . ?
C13B O1B CaB 126.29(11) . . ?
C14B O1B CaB 117.08(11) . . ?
C16B O2B C15B 112.65(14) . . ?
C16B O2B CaB 130.37(11) . . ?
C15B O2B CaB 106.90(10) . . ?
C1B N1B C7B 118.22(14) . . ?
C1B N1B CaB 121.33(11) . . ?
C7B N1B CaB 120.44(10) . . ?
N1B C1B C6B 119.57(15) . . ?
N1B C1B C2B 124.43(16) . . ?
C6B C1B C2B 115.81(16) . . ?
C3B C2B C1B 121.36(18) . . ?
C4B C3B C2B 121.45(18) . . ?
C3B C4B C5B 118.58(18) . . ?
C6B C5B C4B 120.60(19) . . ?
C5B C6B C1B 122.14(18) . . ?
C12B C7B C8B 116.43(18) . . ?
C12B C7B N1B 122.77(17) . . ?
C8B C7B N1B 120.62(17) . . ?
C9B C8B C7B 121.3(2) . . ?
C10B C9B C8B 121.1(2) . . ?
C9B C10B C11B 118.7(2) . . ?
C10B C11B C12B 121.0(2) . . ?
C11B C12B C7B 121.5(2) . . ?
O1B C14B C15B 107.74(16) . . ?
O2B C15B C14B 108.30(16) . . ?
O2B C15B CaB 47.07(8) . . ?
C14B C15B CaB 84.14(11) . . ?
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
CaA N1A 2.3692(15) . ?
CaA N1A 2.3693(15) 2_656 ?
CaA O2A 2.4463(12) 2_656 ?
CaA O2A 2.4464(12) . ?
CaA O1A 2.4769(13) 2_656 ?
CaA O1A 2.4769(13) . ?
CaA C1A 3.1737(18) . ?
CaA C1A 3.1737(18) 2_656 ?
O1A C14A 1.421(2) . ?
O1A C13A 1.434(2) . ?
O2A C16A 1.432(2) . ?
O2A C15A 1.445(2) . ?
N1A C7A 1.375(2) . ?
N1A C1A 1.400(2) . ?
C1A C6A 1.399(3) . ?
C1A C2A 1.413(3) . ?
C2A C3A 1.384(3) . ?
C3A C4A 1.389(3) . ?
C4A C5A 1.380(3) . ?
C5A C6A 1.388(3) . ?
C7A C12A 1.410(3) . ?
C7A C8A 1.417(3) . ?
C8A C9A 1.385(3) . ?
C9A C10A 1.384(3) . ?
C10A C11A 1.391(3) . ?
C11A C12A 1.380(3) . ?
C14A C15A 1.500(3) . ?
CaB N1B 2.3810(14) . ?
CaB N1B 2.3811(14) 2 ?
CaB O2B 2.4079(12) . ?
CaB O2B 2.4079(12) 2 ?
CaB O1B 2.4390(12) . ?
CaB O1B 2.4390(12) 2 ?
CaB C15B 3.1467(19) . ?
CaB C15B 3.1467(19) 2 ?
O1B C13B 1.430(2) . ?
O1B C14B 1.430(2) . ?
O2B C16B 1.435(2) . ?
O2B C15B 1.443(2) . ?
N1B C1B 1.376(2) . ?
N1B C7B 1.400(2) . ?
C1B C6B 1.409(3) . ?
C1B C2B 1.418(2) . ?
C2B C3B 1.384(3) . ?
C3B C4B 1.376(3) . ?
C4B C5B 1.391(3) . ?
C5B C6B 1.382(3) . ?
C7B C12B 1.392(3) . ?
C7B C8B 1.395(3) . ?
C8B C9B 1.390(3) . ?
C9B C10B 1.364(3) . ?
C10B C11B 1.370(3) . ?
C11B C12B 1.388(3) . ?
C14B C15B 1.491(3) . ?
