#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:43:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179074 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303621.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_4303621
loop_
_publ_author_name
'Melanie R. Hauser'
'Kenneth M. Doxsee'
'Håkon Hope'
_publ_contact_author_address
;    Department of Chemistry
    University of Oregon
    Eugene, OR
    USA
    97403
;
_publ_contact_author_email       doxsee@uoregon.edu
_publ_contact_author_name        'Kenneth M. Doxsee'
_publ_section_title
;
Calcium Complexation by Corticosteroids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10780
_journal_page_last               10788
_journal_paper_doi               10.1021/ic901670r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H22 Ca O7, H2 O, 2(Cl)'
_chemical_formula_sum            'C16 H24 Ca Cl2 O8'
_chemical_formula_weight         455.33
_chemical_name_common            'phenacyl alcohol, calcium complex'
_chemical_name_systematic
;
2'-hydroxyacetophenone, calcium complex
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.374(3)
_cell_length_b                   23.314(5)
_cell_length_c                   12.458(3)
_cell_measurement_reflns_used    1571
_cell_measurement_temperature    120
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      0.0
_cell_volume                     2141.7(11)
_computing_data_collection       'Siemens SHELXTL PLUS (VMS)'
_computing_structure_refinement  'Full-Matrix Least Squares'
_computing_structure_solution    'Direct Methods'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Siemens R3m/V'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2467
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.6
_exptl_absorpt_correction_T_min  0.3
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Parkin, J. Appl. Cryst. 1995, 28, 53-56'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.42
_refine_diff_density_min         -0
_refine_ls_goodness_of_fit_all   0.64
_refine_ls_goodness_of_fit_ref   0.64
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2467
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w⁻¹=σ²(F)+0.0239F²
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1424
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                1571
_reflns_number_total             2467
_reflns_threshold_expression     F>6xσ(F)
_cod_data_source_file            ic901670r_si_001_1.cif
_cod_data_source_block           phenacyl_alcohol_calcium_complex
_cod_original_cell_volume        2141.9(11)
_cod_database_code               4303621
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
x,-y,1/2+z
-x,-y,-z
-x,y,1/2-z
1/2-x,1/2-y,1/2+z
1/2-x,1/2+y,z
1/2+x,1/2+y,1/2-z
1/2+x,1/2-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
Ca 0.5000 0.4351(1) 0.7500 0.021(1) Uiso
Cl 0.2171(1) 0.5884(1) 0.5834(1) 0.027(1) Uiso
C1 0.3618(5) 0.3670(1) 0.5357(3) 0.022(1) Uiso
C2 0.2934(5) 0.4265(1) 0.5071(2) 0.022(1) Uiso
C3 0.3390(5) 0.3203(1) 0.4575(3) 0.021(1) Uiso
C4 0.2611(5) 0.3301(2) 0.3562(3) 0.028(1) Uiso
C5 0.2437(5) 0.2851(2) 0.2835(3) 0.031(1) Uiso
C6 0.2978(5) 0.2303(2) 0.3121(3) 0.034(1) Uiso
C7 0.3746(5) 0.2198(2) 0.4134(3) 0.032(1) Uiso
C8 0.3959(5) 0.2653(1) 0.4848(3) 0.025(1) Uiso
O1 0.4316(3) 0.3594(1) 0.6240(2) 0.024(1) Uiso
O2 0.3379(4) 0.4639(1) 0.5929(2) 0.030(1) Uiso
O3 0.5000 0.5393(1) 0.7500 0.030(1) Uiso
O4 0.7820(4) 0.4333(1) 0.6652(2) 0.035(1) Uiso
O5 0.0000 0.5174(2) 0.7500 0.033(1) Uiso
H2A 0.3384 0.4432 0.4345 0.021 Uiso
H2B 0.1568 0.4237 0.4969 0.043 Uiso
H4 0.2238 0.3710 0.3385 0.031 Uiso
H5 0.1856 0.2956 0.2215 0.034 Uiso
H6 0.2880 0.1958 0.2624 0.022 Uiso
H7 0.4165 0.1808 0.4280 0.032 Uiso
H8 0.4477 0.2584 0.5557 0.041 Uiso
H2 0.2874 0.4961 0.5744 0.035 Uiso
H3A 0.4442 0.5604 0.7131 0.048 Uiso
H4A 0.7934 0.4278 0.5984 0.042 Uiso
H4B 0.8662 0.4584 0.6792 0.059 Uiso
H5A 0.0503 0.5405 0.7059 0.044 Uiso
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'
Cl Cl 0.1484 0.1585 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca O2 64.4(1) . . . ?
O2 Ca O3 73.7(1) . . . ?
O2 Ca O4 94.6(1) . . . ?
O1 Ca O1 86.1(1) . . . ?
O3 Ca O1 137.0(1) . . . ?
O1 Ca O2 64.44(8) . . . ?
O3 Ca O2 73.7(1) . . . ?
O4 Ca O4 177.9(1) . . . ?
O2 Ca O4 94.6(1) . . . ?
C2 C1 O1 118.8(3) . . . ?
C1 C2 O2 107.9(3) . . . ?
C1 C3 C8 119.1(3) . . . ?
C3 C4 C5 120.0(3) . . . ?
C5 C6 C7 120.6(3) . . . ?
C3 C8 C7 120.8(3) . . . ?
Ca O2 C2 124.1(2) . . . ?
O1 Ca O3 137.0(1) . . . ?
O1 Ca O4 83.0(1) . . . ?
O3 Ca O4 91.1(1) . . . ?
O2 Ca O2 147.4(1) . . . ?
O3 Ca O4 91.1(1) . . . ?
O1 Ca O4 83.0(1) . . . ?
C2 C1 C3 118.9(3) . . . ?
C3 C1 O1 122.3(3) . . . ?
C1 C3 C4 121.4(3) . . . ?
C4 C3 C8 119.5(3) . . . ?
C4 C5 C6 120.0(3) . . . ?
C6 C7 C8 119.0(3) . . . ?
Ca O1 C1 124.4(2) . . . ?
H2A C2 H2B 103.39 . . . ?
H3A O3 H3A 102.87 . . . ?
H4A O4 H4B 103.18 . . . ?
H5A O5 H5A 101.82 . . . ?
Ca O2 H2 132.39 . . . ?
C2 O2 H2 103.42 . . . ?
O2 C2 H2A 110.60 . . . ?
O2 C2 H2B 111.27 . . . ?
C1 C2 H2A 116.13 . . . ?
C1 C2 H2B 107.43 . . . ?
C3 C4 H4 117.25 . . . ?
C5 C4 H4 122.74 . . . ?
C4 C5 H5 112.96 . . . ?
C6 C5 H5 126.71 . . . ?
C5 C6 H6 123.51 . . . ?
C7 C6 H6 115.94 . . . ?
C6 C7 H7 117.18 . . . ?
C8 C7 H7 123.63 . . . ?
C7 C8 H8 119.77 . . . ?
C3 C8 H8 119.43 . . . ?
Ca O3 H3A 128.57 . . . ?
Ca O4 H4A 122.46 . . . ?
Ca O4 H4B 122.19 . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca O1 2.415(3) . . ?
Ca O3 2.429(4) . . ?
Ca O1 2.415(3) . . ?
Ca O4 2.333(3) . . ?
C1 C3 1.471(5) . . ?
C2 O2 1.417(4) . . ?
C3 C8 1.391(4) . . ?
C5 C6 1.384(5) . . ?
C7 C8 1.393(5) . . ?
Ca O2 2.389(3) . . ?
Ca O4 2.333(3) . . ?
Ca O2 2.389(3) . . ?
C1 C2 1.519(5) . . ?
C1 O1 1.227(4) . . ?
C3 C4 1.404(5) . . ?
C4 C5 1.392(5) . . ?
C6 C7 1.406(5) . . ?
O2 H2 0.869 . . ?
C2 H2A 1.039 . . ?
C2 H2B 1.017 . . ?
C4 H4 1.017 . . ?
C5 H5 0.917 . . ?
C6 H6 1.018 . . ?
C7 H7 0.977 . . ?
C8 H8 0.976 . . ?
O3 H3A 0.789 . . ?
O4 H4A 0.846 . . ?
O4 H4B 0.871 . . ?
O5 H5A 0.854 . . ?
