{Ca(OH~2~)~3~[Ca(DOTA)].7.7H~2~O}~<i>n~</i>
Anderson, O. P.; Reibenspies, J. H.; Acta Crystallographica Section C 52 (1996) 792–795; doi:10.1107/S0108270195013916

data_2004724
_publ_contact_author
;'Dr. Joseph H. Reibenspies
Department of Chemistry
Texas A & M University
College Station, Texas 77843
U.S.A.
;
_publ_section_title
;
 {Ca(OH~2~)~3~[Ca(DOTA)].7.7H~2~O}~<i>n~</i>
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              792
_journal_page_last               795
_journal_paper_doi               10.1107/S0108270195013916
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C16 H30 Ca2 N4 O11,7.7(H2 O)'
_chemical_formula_sum            'C16 H45.4 Ca2 N4 O18.7'
_chemical_formula_weight         673.1
_chemical_name_systematic
;
catena-triaquocalcium-1,4,7,10-tetraazacyclododecane-
N,N',N",N'''-tetraaceto calcium hydrate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 134.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.109(2)
_cell_length_b                   18.557(4)
_cell_length_c                   18.436(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      10.1
_cell_volume                     6090(3)
_computing_data_collection       'P3 (Siemens, 1982)'
_computing_data_reduction        'XTAPE (Siemens, 1990)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens R3m/E'
_diffrn_measurement_method       \q-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4509
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       needle
_exptl_crystal_F_000             2871
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.615
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.317
_refine_ls_goodness_of_fit_obs   1.483
_refine_ls_hydrogen_treatment
' H atoms riding, C-H 0.96\%A, water H atoms not allowed for'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         4364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.273
_refine_ls_restrained_S_obs      1.483
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_obs          0.0681
_refine_ls_shift/esd_max         -0.148
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^) + (0.0918P)^2^ + 12.0614P]
where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.2066
_refine_ls_wR_factor_obs         0.1999
_reflns_number_observed          3108
_reflns_number_total             4364
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1080.cif
_cod_data_source_block           cado
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H45.40 Ca2 N4 O18.7'
_cod_database_code               2004724