Homoleptic Poly(nitrato) Complexes of Group 14 Stable at Ambient Conditions.
Portius, Peter; Peerless, Benjamin; Davis, Martin; Campbell, Rory; Inorganic chemistry 55 (2016) 8976–8984; doi:10.1021/acs.inorgchem.6b01455

data_4348637
_publ_section_title
;
 Homoleptic Poly(nitrato) Complexes of Group 14 Stable at Ambient
 Conditions.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8976
_journal_page_last               8984
_journal_paper_doi               10.1021/acs.inorgchem.6b01455
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '2(C36 H30 N P2), N6 O18 Si'
_chemical_formula_sum            'C72 H60 N8 O18 P4 Si'
_chemical_formula_weight         1477.25
_chemical_name_common            (PPN)2Si(NO3)6
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                85.964(2)
_cell_angle_beta                 77.737(2)
_cell_angle_gamma                83.246(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1566(5)
_cell_length_b                   15.5873(6)
_cell_length_c                   17.2414(8)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4200
_cell_measurement_theta_min      2.1713
_cell_volume                     3427.4(2)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47638
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9958
_exptl_absorpt_correction_T_min  0.9384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         15364
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0392P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9422
_reflns_number_total             15364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01455_si_002.cif
_cod_data_source_block           ch1ppx199_0m
_cod_database_code               4348637
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014-3
_shelx_res_checksum              84684
_shelx_hkl_checksum              41041