#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320972.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_4320972
loop_
_publ_author_name
'Dirk Pfeiffer'
'Mary Jane Heeg'
'Charles H. Winter'
_publ_section_title
;
 Synthesis and Characterization of Calcium Complexes Containing
 η2-Pyrazolato Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2377
_journal_page_last               2384
_journal_paper_doi               10.1021/ic991049c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C28 H54 Ca N6'
_chemical_formula_weight         514.85
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 127.4000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.4089(10)
_cell_length_b                   15.4992(4)
_cell_length_c                   19.1660(6)
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    295(2)
_cell_volume                     6704.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.067
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33813
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00006(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.975
_refine_ls_goodness_of_fit_obs   1.204
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_restrained_S_obs      1.204
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_obs          0.0736
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0992P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2080
_refine_ls_wR_factor_obs         0.1656
_reflns_number_observed          3026
_reflns_number_total             6949
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991049c_2.cif
_cod_data_source_block           capy(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0992P)^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^)+(0.0992P)^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_database_code               4320972
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ca1 Ca 0.0000 0.73489(6) 0.2500 0.0547(3) Uani 1 d S .
Ca2 Ca 0.0000 0.23393(6) 0.2500 0.0550(3) Uani 1 d S .
N1 N -0.07308(12) 0.6560(2) 0.1261(2) 0.0548(7) Uani 1 d . .
N2 N -0.09428(12) 0.6744(2) 0.1736(2) 0.0520(7) Uani 1 d . .
C1 C -0.1170(2) 0.6185(2) 0.0509(2) 0.0557(9) Uani 1 d . .
C2 C -0.1665(2) 0.6122(2) 0.0493(2) 0.0602(9) Uani 1 d . .
H2 H -0.2030(2) 0.5885(2) 0.0048(2) 0.072 Uiso 1 calc R .
C3 C -0.1504(2) 0.6481(2) 0.1268(2) 0.0506(8) Uani 1 d . .
C4 C -0.1100(2) 0.5930(3) -0.0182(2) 0.0711(11) Uani 1 d . .
C5 C -0.1309(3) 0.5008(3) -0.0475(3) 0.136(2) Uani 1 d . .
H5A H -0.1239(15) 0.4836(9) -0.0885(18) 0.163 Uiso 1 calc R .
H5B H -0.1726(4) 0.4972(5) -0.0750(20) 0.163 Uiso 1 calc R .
H5C H -0.1096(11) 0.4633(4) 0.0027(5) 0.163 Uiso 1 calc R .
C6 C -0.0453(2) 0.5956(3) 0.0176(3) 0.109(2) Uani 1 d . .
H6A H -0.0421(3) 0.5766(17) -0.0270(7) 0.131 Uiso 1 calc R .
H6B H -0.0224(3) 0.5583(13) 0.0677(11) 0.131 Uiso 1 calc R .
H6C H -0.0307(4) 0.6536(4) 0.0345(16) 0.131 Uiso 1 calc R .
C7 C -0.1467(2) 0.6517(4) -0.0965(3) 0.144(2) Uani 1 d . .
H7A H -0.1423(14) 0.6353(16) -0.1405(11) 0.173 Uiso 1 calc R .
H7B H -0.1337(10) 0.7102(5) -0.0788(6) 0.173 Uiso 1 calc R .
H7C H -0.1876(3) 0.6471(18) -0.1201(15) 0.173 Uiso 1 calc R .
C8 C -0.1854(2) 0.6594(2) 0.1610(2) 0.0590(9) Uani 1 d . .
C9 C -0.1829(2) 0.7527(3) 0.1872(3) 0.107(2) Uani 1 d . .
H9A H -0.2059(10) 0.7593(5) 0.2084(18) 0.129 Uiso 1 calc R .
H9B H -0.1988(11) 0.7893(3) 0.1370(5) 0.129 Uiso 1 calc R .
H9C H -0.1425(3) 0.7686(6) 0.2326(13) 0.129 Uiso 1 calc R .
C10 C -0.2508(2) 0.6398(4) 0.0897(3) 0.131(2) Uani 1 d . .
H10A H -0.2728(3) 0.6506(19) 0.1119(7) 0.157 Uiso 1 calc R .
H10B H -0.2553(2) 0.5804(6) 0.0726(14) 0.157 Uiso 1 calc R .
H10C H -0.2655(4) 0.6760(14) 0.0397(9) 0.157 Uiso 1 calc R .
C11 C -0.1610(3) 0.6036(4) 0.2398(3) 0.141(2) Uani 1 d . .
H11A H -0.1836(11) 0.6120(18) 0.2613(15) 0.169 Uiso 1 calc R .
H11B H -0.1204(6) 0.6189(16) 0.2849(9) 0.169 Uiso 1 calc R .
H11C H -0.1632(15) 0.5442(4) 0.2239(6) 0.169 Uiso 1 calc R .
N3 N -0.0273(2) 0.8686(2) 0.1564(2) 0.0798(10) Uani 1 d . .
C12 C -0.0052(2) 0.8630(3) 0.1061(4) 0.121(2) Uani 1 d . .
H12A H 0.0373(2) 0.8602(18) 0.1453(4) 0.146 Uiso 1 calc R .
H12B H -0.0174(11) 0.9130(10) 0.0692(14) 0.146 Uiso 1 calc R .
H12C H -0.0206(10) 0.8120(11) 0.0703(14) 0.146 Uiso 1 calc R .
C13 C -0.0920(2) 0.8722(3) 0.0962(3) 0.116(2) Uani 1 d . .
H13A H -0.1073(2) 0.8683(19) 0.1291(4) 0.139 Uiso 1 calc R .
H13B H -0.1068(2) 0.8249(11) 0.0557(12) 0.139 Uiso 1 calc R .
H13C H -0.1044(2) 0.9256(9) 0.0644(14) 0.139 Uiso 1 calc R .
C14 C -0.0014(3) 0.9454(3) 0.2123(3) 0.123(2) Uani 1 d . .
H14A H 0.0384(3) 0.9526(3) 0.2301(3) 0.148 Uiso 1 calc R .
H14B H -0.0243(3) 0.9953(3) 0.1771(3) 0.148 Uiso 1 calc R .
N4 N -0.08503(13) 0.1523(2) 0.1948(2) 0.0599(8) Uani 1 d . .
N5 N -0.08192(13) 0.1688(2) 0.1268(2) 0.0593(8) Uani 1 d . .
C15 C -0.1368(2) 0.1145(2) 0.1614(3) 0.0649(10) Uani 1 d . .
C16 C -0.1680(2) 0.1056(2) 0.0717(3) 0.0791(12) Uani 1 d . .
H16 H -0.2053(2) 0.0813(2) 0.0324(3) 0.095 Uiso 1 calc R .
C17 C -0.1321(2) 0.1402(2) 0.0524(2) 0.0680(11) Uani 1 d . .
C18 C -0.1559(2) 0.0906(2) 0.2171(3) 0.0809(12) Uani 1 d . .
C19 C -0.1761(2) -0.0030(3) 0.2008(4) 0.117(2) Uani 1 d . .
H19A H -0.1910(13) -0.0164(6) 0.2331(16) 0.140 Uiso 1 calc R .
H19B H -0.1433(4) -0.0401(3) 0.2199(18) 0.140 Uiso 1 calc R .
H19C H -0.2069(9) -0.0117(5) 0.1393(5) 0.140 Uiso 1 calc R .
C20 C -0.1055(2) 0.1011(3) 0.3146(3) 0.115(2) Uani 1 d . .
H20A H -0.1180(5) 0.0810(17) 0.3483(3) 0.139 Uiso 1 calc R .
H20B H -0.0947(9) 0.1609(4) 0.3274(5) 0.139 Uiso 1 calc R .
H20C H -0.0719(5) 0.0681(15) 0.3296(5) 0.139 Uiso 1 calc R .
C21 C -0.2069(3) 0.1493(4) 0.1930(4) 0.167(3) Uani 1 d . .
H21A H -0.1936(5) 0.2081(5) 0.2054(25) 0.200 Uiso 1 calc R .
H21B H -0.2202(13) 0.1334(18) 0.2268(20) 0.200 Uiso 1 calc R .
H21C H -0.2390(7) 0.1433(20) 0.1315(8) 0.200 Uiso 1 calc R .
C22 C -0.1417(2) 0.1516(3) -0.0339(3) 0.0898(13) Uani 1 d . .
C23 C -0.1343(3) 0.2443(3) -0.0470(4) 0.169(3) Uani 1 d . .
H23A H -0.1473(19) 0.2526(6) -0.1059(10) 0.202 Uiso 1 calc R .
H23B H -0.0933(4) 0.2602(8) -0.0062(20) 0.202 Uiso 1 calc R .
H23C H -0.1576(15) 0.2797(4) -0.0373(28) 0.202 Uiso 1 calc R .
C24 C -0.2029(3) 0.1240(5) -0.1100(3) 0.180(3) Uani 1 d . .
H24A H -0.2316(3) 0.1533(21) -0.1072(16) 0.216 Uiso 1 calc R .
H24B H -0.2069(6) 0.0628(6) -0.1073(16) 0.216 Uiso 1 calc R .
H24C H -0.2095(8) 0.1384(26) -0.1640(3) 0.216 Uiso 1 calc R .
C25 C -0.0977(3) 0.0997(5) -0.0342(4) 0.178(3) Uani 1 d . .
H25A H -0.0584(3) 0.1136(21) 0.0168(17) 0.214 Uiso 1 calc R .
H25B H -0.1012(15) 0.1125(23) -0.0862(16) 0.214 Uiso 1 calc R .
H25C H -0.1051(12) 0.0394(4) -0.0333(30) 0.214 Uiso 1 calc R .
N6 N -0.0565(2) 0.3683(2) 0.2344(2) 0.0761(9) Uani 1 d . .
C26 C -0.0505(2) 0.3687(3) 0.3142(3) 0.123(2) Uani 1 d . .
H26A H -0.0097(3) 0.3594(19) 0.3632(4) 0.147 Uiso 1 calc R .
H26B H -0.0744(10) 0.3237(13) 0.3123(9) 0.147 Uiso 1 calc R .
H26C H -0.0633(13) 0.4235(8) 0.3207(11) 0.147 Uiso 1 calc R .
C27 C -0.1190(2) 0.3652(3) 0.1597(3) 0.120(2) Uani 1 d . .
H27A H -0.1228(2) 0.3584(19) 0.1066(4) 0.144 Uiso 1 calc R .
H27B H -0.1379(3) 0.4178(8) 0.1568(12) 0.144 Uiso 1 calc R .
H27C H -0.1374(3) 0.3173(12) 0.1662(10) 0.144 Uiso 1 calc R .
C28 C -0.0309(2) 0.4459(2) 0.2264(4) 0.112(2) Uani 1 d . .
H28A H -0.0490(2) 0.4546(2) 0.1648(4) 0.134 Uiso 1 calc R .
H28B H -0.0416(2) 0.4948(2) 0.2457(4) 0.134 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'
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
N2 Ca1 N2 132.55(13) . 2 ?
N2 Ca1 N1 34.73(8) . . ?
N2 Ca1 N1 113.62(9) 2 . ?
N2 Ca1 N1 113.62(9) . 2 ?
N2 Ca1 N1 34.73(8) 2 2 ?
N1 Ca1 N1 116.87(13) . 2 ?
N2 Ca1 N3 120.98(10) . 2 ?
N2 Ca1 N3 98.23(10) 2 2 ?
N1 Ca1 N3 148.07(10) . 2 ?
N1 Ca1 N3 90.42(10) 2 2 ?
N2 Ca1 N3 98.23(10) . . ?
N2 Ca1 N3 120.98(10) 2 . ?
N1 Ca1 N3 90.42(10) . . ?
N1 Ca1 N3 148.07(11) 2 . ?
N3 Ca1 N3 70.3(2) 2 . ?
N5 Ca2 N5 128.15(14) . 2 ?
N5 Ca2 N4 34.64(9) . . ?
N5 Ca2 N4 110.41(10) 2 . ?
N5 Ca2 N4 110.41(10) . 2 ?
N5 Ca2 N4 34.64(9) 2 2 ?
N4 Ca2 N4 114.36(13) . 2 ?
N5 Ca2 N6 130.74(11) . 2 ?
N5 Ca2 N6 93.78(11) 2 2 ?
N4 Ca2 N6 154.95(11) . 2 ?
N4 Ca2 N6 89.13(10) 2 2 ?
N5 Ca2 N6 93.78(11) . . ?
N5 Ca2 N6 130.74(11) 2 . ?
N4 Ca2 N6 89.13(10) . . ?
N4 Ca2 N6 154.95(11) 2 . ?
N6 Ca2 N6 69.47(15) 2 . ?
C1 N1 N2 107.6(3) . . ?
C1 N1 Ca1 174.2(2) . . ?
N2 N1 Ca1 72.4(2) . . ?
C3 N2 N1 108.3(2) . . ?
C3 N2 Ca1 173.9(2) . . ?
N1 N2 Ca1 72.8(2) . . ?
N1 C1 C2 108.9(3) . . ?
N1 C1 C4 121.7(3) . . ?
C2 C1 C4 129.4(3) . . ?
C3 C2 C1 106.3(3) . . ?
N2 C3 C2 109.0(3) . . ?
N2 C3 C8 120.7(3) . . ?
C2 C3 C8 130.3(3) . . ?
C7 C4 C1 109.6(3) . . ?
C7 C4 C5 108.8(4) . . ?
C1 C4 C5 109.8(3) . . ?
C7 C4 C6 110.5(4) . . ?
C1 C4 C6 111.4(3) . . ?
C5 C4 C6 106.7(4) . . ?
C11 C8 C3 110.5(3) . . ?
C11 C8 C9 108.5(4) . . ?
C3 C8 C9 110.3(3) . . ?
C11 C8 C10 110.8(4) . . ?
C3 C8 C10 110.8(3) . . ?
C9 C8 C10 105.8(4) . . ?
C12 N3 C13 109.0(4) . . ?
C12 N3 C14 108.0(4) . . ?
C13 N3 C14 112.3(4) . . ?
C12 N3 Ca1 110.7(3) . . ?
C13 N3 Ca1 106.7(2) . . ?
C14 N3 Ca1 110.2(2) . . ?
C14 C14 N3 116.4(4) 2 . ?
C15 N4 N5 108.2(3) . . ?
C15 N4 Ca2 173.3(2) . . ?
N5 N4 Ca2 71.7(2) . . ?
C17 N5 N4 107.8(3) . . ?
C17 N5 Ca2 173.3(2) . . ?
N4 N5 Ca2 73.6(2) . . ?
N4 C15 C16 109.2(4) . . ?
N4 C15 C18 122.3(4) . . ?
C16 C15 C18 128.4(4) . . ?
C15 C16 C17 105.9(4) . . ?
N5 C17 C16 108.9(3) . . ?
N5 C17 C22 119.5(4) . . ?
C16 C17 C22 131.6(4) . . ?
C15 C18 C19 110.1(4) . . ?
C15 C18 C20 111.6(3) . . ?
C19 C18 C20 108.1(4) . . ?
C15 C18 C21 108.8(4) . . ?
C19 C18 C21 109.6(4) . . ?
C20 C18 C21 108.7(4) . . ?
C25 C22 C23 108.4(5) . . ?
C25 C22 C24 108.8(5) . . ?
C23 C22 C24 107.9(5) . . ?
C25 C22 C17 110.3(4) . . ?
C23 C22 C17 110.2(4) . . ?
C24 C22 C17 111.1(4) . . ?
C26 N6 C27 109.6(4) . . ?
C26 N6 C28 111.3(4) . . ?
C27 N6 C28 108.1(4) . . ?
C26 N6 Ca2 102.8(3) . . ?
C27 N6 Ca2 113.3(2) . . ?
C28 N6 Ca2 111.7(2) . . ?
C28 C28 N6 116.1(3) 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
Ca1 N2 2.331(3) . ?
Ca1 N2 2.331(3) 2 ?
Ca1 N1 2.336(3) . ?
Ca1 N1 2.336(3) 2 ?
Ca1 N3 2.535(3) 2 ?
Ca1 N3 2.535(3) . ?
Ca2 N5 2.310(3) . ?
Ca2 N5 2.310(3) 2 ?
Ca2 N4 2.335(3) . ?
Ca2 N4 2.335(3) 2 ?
Ca2 N6 2.534(3) 2 ?
Ca2 N6 2.534(3) . ?
N1 C1 1.337(4) . ?
N1 N2 1.393(3) . ?
N2 C3 1.333(4) . ?
C1 C2 1.389(5) . ?
C1 C4 1.508(5) . ?
C2 C3 1.379(4) . ?
C3 C8 1.496(4) . ?
C4 C7 1.505(5) . ?
C4 C5 1.519(6) . ?
C4 C6 1.521(5) . ?
C8 C11 1.496(5) . ?
C8 C9 1.518(5) . ?
C8 C10 1.526(5) . ?
N3 C12 1.439(5) . ?
N3 C13 1.461(5) . ?
N3 C14 1.465(5) . ?
C14 C14 1.399(9) 2 ?
N4 C15 1.331(4) . ?
N4 N5 1.383(4) . ?
N5 C17 1.339(4) . ?
C15 C16 1.382(5) . ?
C15 C18 1.508(5) . ?
C16 C17 1.386(5) . ?
C17 C22 1.514(5) . ?
C18 C19 1.521(5) . ?
C18 C20 1.523(6) . ?
C18 C21 1.526(6) . ?
C22 C25 1.488(7) . ?
C22 C23 1.496(6) . ?
C22 C24 1.502(6) . ?
N6 C26 1.433(5) . ?
N6 C27 1.454(5) . ?
N6 C28 1.461(5) . ?
C28 C28 1.406(8) 2 ?
