#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:04:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179739 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/35/7003570.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_7003570
loop_
_publ_author_name
'Gärtner, Martin'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Synthesis and structural variations of substituted phenylamide
 complexes of the heavy alkaline earth metals calcium, strontium and
 barium
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              1574
_journal_page_last               1582
_journal_paper_doi               10.1039/b717267b
_journal_year                    2008
_chemical_formula_sum            'C30 H48 Ca N2 O4'
_chemical_formula_weight         540.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7482(10)
_cell_length_b                   17.8861(11)
_cell_length_c                   20.6278(14)
_cell_measurement_temperature    183(2)
_cell_volume                     6179.3(7)
_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 0.955
_diffrn_measured_fraction_theta_max 0.939
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19352
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9884
_exptl_absorpt_correction_T_min  0.9434
_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    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0600
_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)+(0.0499P)²+3.7556P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                4035
_reflns_number_total             6636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717267b.txt
_cod_data_source_block           FO3228
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7003570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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_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
Ca Ca 0.28553(3) 0.05638(3) 0.13380(2) 0.02352(14) Uani 1 1 d . . .
O1 O 0.14155(11) 0.06628(11) 0.13461(10) 0.0381(5) Uani 1 1 d . . .
O2 O 0.26965(10) -0.04516(10) 0.21093(8) 0.0315(4) Uani 1 1 d . . .
O3 O 0.42658(10) 0.03914(10) 0.13502(8) 0.0291(4) Uani 1 1 d . . .
O4 O 0.29760(11) 0.16267(10) 0.06359(8) 0.0342(5) Uani 1 1 d . . .
N1 N 0.29688(12) 0.13562(12) 0.22733(10) 0.0274(5) Uani 1 1 d . . .
N2 N 0.27370(13) -0.02353(13) 0.03918(10) 0.0306(5) Uani 1 1 d . . .
C1 C 0.35036(15) 0.18849(14) 0.24689(12) 0.0264(6) Uani 1 1 d . . .
C2 C 0.41708(15) 0.20517(15) 0.20714(13) 0.0312(6) Uani 1 1 d . . .
H2A H 0.4243 0.1778 0.1681 0.037 Uiso 1 1 calc R . .
C3 C 0.47153(16) 0.25926(17) 0.22288(15) 0.0411(7) Uani 1 1 d . . .
H3A H 0.5155 0.2681 0.1948 0.049 Uiso 1 1 calc R . .
C4 C 0.46372(17) 0.30167(18) 0.27931(16) 0.0441(8) Uani 1 1 d . . .
H4A H 0.5012 0.3397 0.2899 0.053 Uiso 1 1 calc R . .
C5 C 0.39992(18) 0.28647(17) 0.31911(14) 0.0392(7) Uani 1 1 d . . .
H5A H 0.3933 0.3148 0.3577 0.047 Uiso 1 1 calc R . .
C6 C 0.34510(16) 0.23126(16) 0.30468(13) 0.0323(6) Uani 1 1 d . . .
H6A H 0.3028 0.2217 0.3342 0.039 Uiso 1 1 calc R . .
C7 C 0.23127(16) 0.12361(16) 0.27241(13) 0.0329(6) Uani 1 1 d . . .
H7A H 0.2526 0.1083 0.3146 0.049 Uiso 1 1 calc R . .
H7B H 0.1961 0.0844 0.2556 0.049 Uiso 1 1 calc R . .
H7C H 0.2009 0.1701 0.2774 0.049 Uiso 1 1 calc R . .
C8 C 0.31351(15) -0.08570(15) 0.01976(12) 0.0270(6) Uani 1 1 d . . .
C9 C 0.37274(15) -0.11777(15) 0.06079(13) 0.0282(6) Uani 1 1 d . . .
H9A H 0.3827 -0.0952 0.1017 0.034 Uiso 1 1 calc R . .
C10 C 0.41606(15) -0.17992(16) 0.04376(14) 0.0329(6) Uani 1 1 d . . .
H10A H 0.4553 -0.1985 0.0728 0.039 Uiso 1 1 calc R . .
C11 C 0.40373(18) -0.21634(17) -0.01519(15) 0.0391(7) Uani 1 1 d . . .
H11A H 0.4336 -0.2595 -0.0268 0.047 Uiso 1 1 calc R . .
C12 C 0.34617(18) -0.18707(17) -0.05613(14) 0.0395(7) Uani 1 1 d . . .
H12A H 0.3368 -0.2106 -0.0967 0.047 Uiso 1 1 calc R . .
C13 C 0.30185(16) -0.12459(16) -0.03972(13) 0.0333(6) Uani 1 1 d . . .
H13A H 0.2624 -0.1071 -0.0691 0.040 Uiso 1 1 calc R . .
C14 C 0.21443(18) 0.00340(18) -0.00715(14) 0.0408(7) Uani 1 1 d . . .
H14A H 0.1745 -0.0357 -0.0147 0.061 Uiso 1 1 calc R . .
H14B H 0.2408 0.0159 -0.0481 0.061 Uiso 1 1 calc R . .
H14C H 0.1882 0.0480 0.0103 0.061 Uiso 1 1 calc R . .
C15 C 0.0958(2) 0.1346(2) 0.1333(2) 0.0728(12) Uani 1 1 d . . .
H15A H 0.0952 0.1578 0.1769 0.087 Uiso 1 1 calc R . .
H15B H 0.1197 0.1704 0.1024 0.087 Uiso 1 1 calc R . .
C16 C 0.0158(2) 0.1160(3) 0.1136(3) 0.1012(18) Uani 1 1 d . . .
H16A H 0.0039 0.1390 0.0710 0.121 Uiso 1 1 calc R . .
H16B H -0.0231 0.1353 0.1456 0.121 Uiso 1 1 calc R . .
C17 C 0.0097(2) 0.0349(3) 0.1091(2) 0.0817(14) Uani 1 1 d . . .
H17A H -0.0005 0.0195 0.0638 0.098 Uiso 1 1 calc R . .
H17B H -0.0347 0.0165 0.1365 0.098 Uiso 1 1 calc R . .
C18 C 0.08756(18) 0.00353(19) 0.13234(16) 0.0472(8) Uani 1 1 d . . .
H18A H 0.0815 -0.0191 0.1759 0.057 Uiso 1 1 calc R . .
H18B H 0.1075 -0.0351 0.1020 0.057 Uiso 1 1 calc R . .
C19 C 0.24566(17) -0.12010(15) 0.19302(13) 0.0326(6) Uani 1 1 d . . .
H19A H 0.2462 -0.1264 0.1453 0.039 Uiso 1 1 calc R . .
H19B H 0.1915 -0.1315 0.2094 0.039 Uiso 1 1 calc R . .
C20 C 0.30754(17) -0.16990(16) 0.22492(14) 0.0372(7) Uani 1 1 d . . .
H20A H 0.3554 -0.1755 0.1971 0.045 Uiso 1 1 calc R . .
H20B H 0.2853 -0.2200 0.2344 0.045 Uiso 1 1 calc R . .
C21 C 0.32749(19) -0.12777(18) 0.28738(15) 0.0441(8) Uani 1 1 d . . .
H21A H 0.3037 -0.1532 0.3254 0.053 Uiso 1 1 calc R . .
H21B H 0.3860 -0.1245 0.2936 0.053 Uiso 1 1 calc R . .
C22 C 0.29154(17) -0.05022(17) 0.27852(12) 0.0353(6) Uani 1 1 d . . .
H22A H 0.2440 -0.0440 0.3065 0.042 Uiso 1 1 calc R . .
H22B H 0.3310 -0.0111 0.2898 0.042 Uiso 1 1 calc R . .
C23 C 0.47945(16) 0.03874(17) 0.07945(13) 0.0350(7) Uani 1 1 d . . .
H23A H 0.4959 0.0902 0.0680 0.042 Uiso 1 1 calc R . .
H23B H 0.4529 0.0157 0.0415 0.042 Uiso 1 1 calc R . .
C24 C 0.55048(16) -0.00704(18) 0.10032(14) 0.0403(7) Uani 1 1 d . . .
H24A H 0.5990 0.0067 0.0757 0.048 Uiso 1 1 calc R . .
H24B H 0.5403 -0.0613 0.0953 0.048 Uiso 1 1 calc R . .
C25 C 0.55756(17) 0.01490(19) 0.17142(15) 0.0443(8) Uani 1 1 d . . .
H25A H 0.5870 -0.0235 0.1964 0.053 Uiso 1 1 calc R . .
H25B H 0.5848 0.0637 0.1764 0.053 Uiso 1 1 calc R . .
C26 C 0.47125(16) 0.01950(17) 0.19267(13) 0.0345(7) Uani 1 1 d . . .
H26A H 0.4530 -0.0292 0.2101 0.041 Uiso 1 1 calc R . .
H26B H 0.4645 0.0581 0.2266 0.041 Uiso 1 1 calc R . .
C27 C 0.28580(16) 0.23894(15) 0.08439(13) 0.0313(6) Uani 1 1 d . . .
H27A H 0.2885 0.2427 0.1322 0.038 Uiso 1 1 calc R . .
H27B H 0.2333 0.2578 0.0697 0.038 Uiso 1 1 calc R . .
C28 C 0.35255(17) 0.28262(17) 0.05349(14) 0.0396(7) Uani 1 1 d . . .
H28A H 0.4004 0.2833 0.0816 0.047 Uiso 1 1 calc R . .
H28B H 0.3359 0.3347 0.0444 0.047 Uiso 1 1 calc R . .
C29 C 0.3686(2) 0.2403(2) -0.00877(16) 0.0526(9) Uani 1 1 d . . .
H29A H 0.3497 0.2693 -0.0467 0.063 Uiso 1 1 calc R . .
H29B H 0.4264 0.2304 -0.0138 0.063 Uiso 1 1 calc R . .
C30 C 0.3230(2) 0.16807(19) -0.00286(14) 0.0522(9) Uani 1 1 d . . .
H30A H 0.2763 0.1682 -0.0322 0.063 Uiso 1 1 calc R . .
H30B H 0.3577 0.1252 -0.0143 0.063 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
O3 Ca O4 91.45(6) . . ?
O3 Ca N1 89.39(7) . . ?
O4 Ca N1 90.61(7) . . ?
O3 Ca O1 176.62(7) . . ?
O4 Ca O1 91.73(7) . . ?
N1 Ca O1 91.73(7) . . ?
O3 Ca N2 90.76(7) . . ?
O4 Ca N2 89.32(7) . . ?
N1 Ca N2 179.84(8) . . ?
O1 Ca N2 88.13(7) . . ?
O3 Ca O2 90.28(6) . . ?
O4 Ca O2 175.84(6) . . ?
N1 Ca O2 85.62(7) . . ?
O1 Ca O2 86.62(6) . . ?
N2 Ca O2 94.45(7) . . ?
C18 O1 C15 109.0(2) . . ?
C18 O1 Ca 124.61(16) . . ?
C15 O1 Ca 126.32(19) . . ?
C22 O2 C19 105.00(19) . . ?
C22 O2 Ca 130.65(16) . . ?
C19 O2 Ca 123.75(15) . . ?
C26 O3 C23 109.44(19) . . ?
C26 O3 Ca 123.53(14) . . ?
C23 O3 Ca 126.75(15) . . ?
C30 O4 C27 105.1(2) . . ?
C30 O4 Ca 130.81(17) . . ?
C27 O4 Ca 123.92(14) . . ?
C1 N1 C7 114.2(2) . . ?
C1 N1 Ca 134.35(16) . . ?
C7 N1 Ca 111.49(16) . . ?
C8 N2 C14 114.3(2) . . ?
C8 N2 Ca 132.83(16) . . ?
C14 N2 Ca 112.81(17) . . ?
N1 C1 C2 119.5(2) . . ?
N1 C1 C6 125.6(2) . . ?
C2 C1 C6 114.9(2) . . ?
C3 C2 C1 122.5(3) . . ?
C2 C3 C4 121.3(3) . . ?
C5 C4 C3 117.6(3) . . ?
C4 C5 C6 122.0(3) . . ?
C5 C6 C1 121.7(3) . . ?
N2 C8 C13 126.0(2) . . ?
N2 C8 C9 119.8(2) . . ?
C13 C8 C9 114.3(2) . . ?
C10 C9 C8 122.8(2) . . ?
C9 C10 C11 121.5(3) . . ?
C12 C11 C10 117.3(3) . . ?
C13 C12 C11 122.0(3) . . ?
C12 C13 C8 122.1(3) . . ?
C16 C15 O1 107.8(3) . . ?
C15 C16 C17 108.2(3) . . ?
C16 C17 C18 106.9(3) . . ?
O1 C18 C17 105.4(3) . . ?
O2 C19 C20 104.1(2) . . ?
C19 C20 C21 103.0(2) . . ?
C22 C21 C20 105.2(2) . . ?
O2 C22 C21 105.9(2) . . ?
O3 C23 C24 105.0(2) . . ?
C23 C24 C25 101.3(2) . . ?
C26 C25 C24 102.6(2) . . ?
O3 C26 C25 105.6(2) . . ?
O4 C27 C28 105.2(2) . . ?
C27 C28 C29 103.4(2) . . ?
C30 C29 C28 105.7(2) . . ?
O4 C30 C29 106.6(2) . . ?
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
Ca O3 2.3825(17) . ?
Ca O4 2.3985(18) . ?
Ca N1 2.402(2) . ?
Ca O1 2.4180(18) . ?
Ca N2 2.427(2) . ?
Ca O2 2.4291(18) . ?
O1 C18 1.442(3) . ?
O1 C15 1.442(4) . ?
O2 C22 1.444(3) . ?
O2 C19 1.447(3) . ?
O3 C26 1.448(3) . ?
O3 C23 1.448(3) . ?
O4 C30 1.439(3) . ?
O4 C27 1.444(3) . ?
N1 C1 1.363(3) . ?
N1 C7 1.455(3) . ?
N2 C8 1.357(3) . ?
N2 C14 1.460(3) . ?
C1 C2 1.418(4) . ?
C1 C6 1.419(4) . ?
C2 C3 1.369(4) . ?
C3 C4 1.396(4) . ?
C4 C5 1.375(4) . ?
C5 C6 1.381(4) . ?
C8 C13 1.424(4) . ?
C8 C9 1.424(4) . ?
C9 C10 1.373(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.385(4) . ?
C12 C13 1.384(4) . ?
C15 C16 1.439(5) . ?
C16 C17 1.458(6) . ?
C17 C18 1.499(5) . ?
C19 C20 1.517(4) . ?
C20 C21 1.529(4) . ?
C21 C22 1.523(4) . ?
C23 C24 1.507(4) . ?
C24 C25 1.523(4) . ?
C25 C26 1.513(4) . ?
C27 C28 1.505(4) . ?
C28 C29 1.515(4) . ?
C29 C30 1.505(5) . ?
