1,3,2-Diheterophospholane complexes: access to new tuneable precursors of phosphanoxyl complexes and P-functional polymers
Brehm, Philipp; Müller-Feyen , Anne Sophie; Schnakenburg, Gregor; Streubel, R.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00027J

data_7709459
_publ_section_title
;
 1,3,2-Diheterophospholane complexes: access to new tuneable precursors of
 phosphanoxyl complexes and P-functional polymers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00027J
_journal_year                    2022
_chemical_formula_moiety         'C19 H29 N2 O7 P W'
_chemical_formula_sum            'C19 H29 N2 O7 P W'
_chemical_formula_weight         612.26
_chemical_name_systematic        PB-211
_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     dual
_audit_creation_date             2020-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                73.319(2)
_cell_angle_beta                 74.659(3)
_cell_angle_gamma                71.740(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2932(3)
_cell_length_b                   10.1104(3)
_cell_length_c                   15.3182(5)
_cell_measurement_reflns_used    23979
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.74
_cell_volume                     1146.66(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19824
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.741
_exptl_absorpt_coefficient_mu    5.148
_exptl_absorpt_correction_T_max  0.6833
_exptl_absorpt_correction_T_min  0.3164
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5246
_reflns_number_total             5540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00027j3.cif
_cod_data_source_block           7a
_cod_database_code               7709459
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.577
_shelx_estimated_absorpt_t_min   0.307
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              41066
_olex2_submission_special_instructions 'No special instructions were received'