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_4348641
_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_sum            'C38 H33 N3 O3 P2'
_chemical_formula_weight         641.61
_chemical_name_common            (PPN)NO3.MeCN
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.867(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8535(8)
_cell_length_b                   12.4798(11)
_cell_length_c                   24.526(2)
_cell_measurement_reflns_used    6959
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5513
_cell_measurement_theta_min      2.8102
_cell_volume                     3251.0(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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  0.0872
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44747
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.624
_diffrn_reflns_theta_min         2.518
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  9865
_exptl_absorpt_correction_T_min  0.9589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0497P)^2^+1.0348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5236
_reflns_number_total             7459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01455_si_002.cif
_cod_data_source_block           ch1ppx138_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348641
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              86508
_shelx_hkl_checksum              6062