The first phosphoramide‒mercury(II) complex with a Cl~2~Hg‒OP[N(C)(C)]~3~ segment
Saneei, Anahid; Pourayoubi, Mehrdad; Crochet, Aurelien; Fromm, Katharina M.; Acta Crystallographica Section C 72 (2016) 230–233; doi:10.1107/S2053229616002394

data_2020423
_publ_section_title
;
 The first phosphoramide--mercury(II) complex with a
 Cl~2~Hg--OP[N(C)(C)]~3~ segment
;
_journal_coeditor_code           LG3182
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              230
_journal_page_last               233
_journal_paper_doi               10.1107/S2053229616002394
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Hg Cl2 (C15 H30 N3 O P)] [Hg Cl2]'
_chemical_formula_moiety         '2(C15 H30 Cl2 Hg N3 O P), Cl2 Hg'
_chemical_formula_sum            'C30 H60 Cl6 Hg3 N6 O2 P2'
_chemical_formula_weight         1413.25
_chemical_name_systematic
;
Dichlorido[tris(piperidin-1-yl)phosphane
oxide-\k<i>O</i>]mercury(II)--dichloridomercury(II) (2/1)
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.337(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1182(15)
_cell_length_b                   10.5995(8)
_cell_length_c                   19.338(3)
_cell_measurement_reflns_used    19807
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      1.06
_cell_volume                     2265.0(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999)
and ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27440
_diffrn_reflns_theta_full        25.204
_diffrn_reflns_theta_max         25.204
_diffrn_reflns_theta_min         2.022
_exptl_absorpt_coefficient_mu    10.601
_exptl_absorpt_correction_T_max  0.1327
_exptl_absorpt_correction_T_min  0.0657
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-SHAPE; Stoe & Cie, 2002)
;
_exptl_crystal_colour            less
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.790
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+5.1731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3336
_reflns_number_total             4041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3182sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020423.cif.'
_cod_database_code               2020423
_cod_database_fobs_code          2020423
_shelx_estimated_absorpt_t_min   0.194
_shelx_estimated_absorpt_t_max   0.417
_shelx_hkl_checksum              70676
_shelx_res_checksum              89092