Tunable Cyclopentane-1,3-diyls Generated by Insertion of Isonitriles into Diphosphadiazanediyls.
Hinz, Alexander; Schulz, Axel; Villinger, Alexander; Journal of the American Chemical Society 137 (2015) 9953–9962; doi:10.1021/jacs.5b05596

data_4124347
_publ_section_title
;
 Tunable Cyclopentane-1,3-diyls Generated by Insertion of Isonitriles into
 Diphosphadiazanediyls.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9953
_journal_page_last               9962
_journal_paper_doi               10.1021/jacs.5b05596
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C49 H52 Cl2 N2 P2'
_chemical_formula_sum            'C49 H52 Cl2 N2 P2'
_chemical_formula_weight         801.76
_chemical_name_systematic
;
 ?
;
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.237(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2499(3)
_cell_length_b                   12.3493(3)
_cell_length_c                   28.5036(8)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.44
_cell_volume                     4310.95(19)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
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_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            57098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         13153
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0557P)^2^+1.3370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8289
_reflns_number_total             13153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05596_si_001.cif
_cod_data_source_block           ah146c
_cod_database_code               4124347
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2013-4
_shelx_res_checksum              90669
_shelx_hkl_checksum              1634