Di-μ-nitrato-bis(μ-octaethyl pyrophosphoramide)bis[aquadinitratocalcium(II)]
Micallef, Duncan; Baisch, Ulrich; Acta Crystallographica Section E 77 (2021) 795–798; doi:10.1107/S205698902100699X

data_2243867
_publ_section_title
;
 Di-\m-nitrato-bis(\m-octaethyl
 pyrophosphoramide)bis[aquadinitratocalcium(II)]
;
_journal_coeditor_code           CQ2040
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              795
_journal_page_last               798
_journal_paper_doi               10.1107/S205698902100699X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ca2 (N O3)4 (C16 H40 N4 O3 P2)2 (H2 O1)2]'
_chemical_formula_moiety         'C32 H84 Ca2 N12 O20 P4'
_chemical_formula_sum            'C32 H84 Ca2 N12 O20 P4'
_chemical_formula_weight         1161.15
_chemical_name_common
;
Diaquatetranitratobis(octaethyl pyrophosphoramide)dicalcium(II)
;
_chemical_name_systematic
'Di-\m-nitrato-\k^3^<i>O</i>,<i>O</i>':<i>O</i>;<i>O</i>:<i>O</i>,<i>O</i>'-bis(\m-octaethyl pyrophosphoramide-\k^2^<i>O</i>:<i>O</i>')bis[aquabis(nitrato-\k^2^<i>O</i>,<i>O</i>')calcium(II)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.707(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6249(7)
_cell_length_b                   15.5774(12)
_cell_length_c                   17.0925(10)
_cell_measurement_reflns_used    18894
_cell_measurement_temperature    150
_cell_measurement_theta_max      50.04
_cell_measurement_theta_min      2.23
_cell_volume                     2809.6(3)
_computing_cell_refinement
;
X-Area Recipe (Stoe & Cie, 2020)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2020)
;
_computing_data_reduction
;
X-Area Integrate (Stoe & Cie, 2020),
X-Red (Stoe & Cie, 2020)
;
_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
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        65.645
_diffrn_reflns_theta_max         65.645
_diffrn_reflns_theta_min         3.851
_diffrn_source                   Genix-Cu
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  0.8272
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED32; Stoe & Cie, 2020),
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.514
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0894P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                4280
_reflns_number_total             4816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cq2040sup1.cif
_cod_data_source_block           I
_cod_database_code               2243867
_shelx_estimated_absorpt_t_min   0.527
_shelx_estimated_absorpt_t_max   0.817
_cod_database_fobs_code 2243867