Crystal structure of aquatris{μ-<i>N</i>-[bis(diethylamino)phosphoryl]-2,2,2-trichloroacetamidato-κ^3^<i>O</i>,<i>O</i>':<i>O</i>}calciumsodium
Shatrava, Iuliia; Gubina, Kateryna; Ovchynnikov, Vladimir; Dyakonenko, Viktoriya; Amirkhanov, Vladimir; Acta Crystallographica Section E 72 (2016) 1683–1686; doi:10.1107/S2056989016017035

data_2241917
_publ_section_title
;
 Crystal structure of
 aquatris{\m-<i>N</i>-[bis(diethylamino)phosphoryl]-2,2,2-trichloroacetamidato-\k^3^<i>O</i>,<i>O</i>':<i>O</i>}calciumsodium
;
_journal_coeditor_code           BG2595
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1683
_journal_page_last               1686
_journal_paper_doi               10.1107/S2056989016017035
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ca Na (C10 H20 Cl3 N3 O2 P)3 (H2 O)]'
_chemical_formula_moiety         'C30 H62 Ca Cl9 N9 Na O7 P3'
_chemical_formula_sum            'C30 H62 Ca Cl9 N9 Na O7 P3'
_chemical_formula_weight         1135.91
_chemical_name_systematic
Aquatris{\m-<i>N</i>-[bis(diethylamino)phosphoryl]-2,2,2-trichloroacetamidato-\k^3^<i>O</i>,<i>O</i>':<i>O</i>}calciumsodium
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.539(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4014(5)
_cell_length_b                   21.8127(10)
_cell_length_c                   18.2427(6)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.0690
_cell_measurement_theta_min      2.9310
_cell_volume                     5242.8(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Agilent Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56299
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.531
_diffrn_reflns_theta_min         2.941
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.534
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         16965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+3.9976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                10752
_reflns_number_total             16965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2595sup1.cif
_cod_data_source_block           I
_cod_database_code               2241917
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.868
_cod_database_fobs_code 2241917