Ring-Opening Polymerization of Cyclic Phosphonates: Access to Inorganic Polymers with a P<sup>V</sup>-O Main Chain.
Arz, Marius I.; Annibale, Vincent T.; Kelly, Nicole L.; Hanna, John V.; Manners, Ian; Journal of the American Chemical Society 141 (2019) 2894–2899; doi:10.1021/jacs.8b13435

data_4128478
_publ_section_title
;
 Ring-Opening Polymerization of Cyclic Phosphonates: Access to Inorganic
 Polymers with a P<sup>V</sup>-O Main Chain.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2894
_journal_page_last               2899
_journal_paper_doi               10.1021/jacs.8b13435
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C27 H33 O6 P3'
_chemical_formula_sum            'C27 H33 O6 P3'
_chemical_formula_weight         546.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.594(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4177(6)
_cell_length_b                   17.2187(17)
_cell_length_c                   9.4319(7)
_cell_measurement_reflns_used    1804
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.28
_cell_volume                     1295.72(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12278
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.650
_diffrn_reflns_theta_min         2.278
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0750 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.8315. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 1460 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.27(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5475
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    0.838
_reflns_Friedel_fraction_max     0.814
_reflns_number_gt                4271
_reflns_number_total             5475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13435_si_002.cif
_cod_data_source_block           1Mes3
_cod_database_code               4128478
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.021) H5(0.021) H7A(0.041) H7B(0.041) H7C(0.041) H8A(0.037)
 H8B(0.037) H8C(0.037) H9A(0.035) H9B(0.035) H9C(0.035) H12(0.023) H14(0.022)
 H16A(0.032) H16B(0.032) H16C(0.032) H17A(0.04) H17B(0.04) H17C(0.04)
 H18A(0.031) H18B(0.031) H18C(0.031) H21(0.025) H23(0.024) H25A(0.037)
 H25B(0.037) H25C(0.037) H26A(0.043) H26B(0.043) H26C(0.043) H27A(0.035)
 H27B(0.035) H27C(0.035)
 Fixed X: H3(0.0645) H5(0.3701) H7A(0.103) H7B(0.1857) H7C(0.2934) H8A(0.1287)
 H8B(0.1049) H8C(-0.0233) H9A(0.6213) H9B(0.7048) H9C(0.5961) H12(0.6549)
 H14(1.0319) H16A(0.3468) H16B(0.3399) H16C(0.4006) H17A(1.0634) H17B(1.0347)
 H17C(0.9159) H18A(1.0072) H18B(0.9041) H18C(0.8268) H21(0.8597) H23(0.9579)
 H25A(0.6281) H25B(0.4767) H25C(0.6215) H26A(1.1569) H26B(1.1578) H26C(1.0577)
 H27A(0.7519) H27B(0.5763) H27C(0.7356)
 Fixed Y: H3(0.566) H5(0.3946) H7A(0.6417) H7B(0.5997) H7C(0.6596) H8A(0.5037)
 H8B(0.4141) H8C(0.4778) H9A(0.3693) H9B(0.4331) H9C(0.3642) H12(0.2027)
 H14(0.3502) H16A(0.2754) H16B(0.291) H16C(0.2084) H17A(0.1954) H17B(0.2498)
 H17C(0.1763) H18A(0.4603) H18B(0.4429) H18C(0.4988) H21(0.8038) H23(0.6562)
 H25A(0.7104) H25B(0.7354) H25C(0.7964) H26A(0.7542) H26B(0.7896) H26C(0.8329)
 H27A(0.5747) H27B(0.5643) H27C(0.5146)
 Fixed Z: H3(0.7228) H5(0.9328) H7A(0.5476) H7B(0.4369) H7C(0.5598)
 H8A(1.0281) H8B(0.9805) H8C(0.8848) H9A(0.9017) H9B(0.8245) H9C(0.7265)
 H12(0.0936) H14(0.2866) H16A(0.0404) H16B(0.2056) H16C(0.1641) H17A(0.2175)
 H17B(0.0738) H17C(0.066) H18A(0.4005) H18B(0.5132) H18C(0.3725) H21(0.4217)
 H23(0.1303) H25A(0.5546) H25B(0.41) H25C(0.4885) H26A(0.2364) H26B(0.3935)
 H26C(0.2411) H27A(-0.0173) H27B(0.0124) H27C(0.1067)
;
_shelx_res_checksum              95104
_shelx_hkl_checksum              14767
_olex2_submission_special_instructions 'No special instructions were received'