Addition-Isomerization Polymerization of Chiral Phosphaalkenes: Observation of Styrene–Phosphaalkene Linkages in a Random Copolymer
Serin, Spencer C.; Dake, Gregory R.; Gates, Derek P.; Macromolecules 49 (2016) 4067–; doi:10.1021/acs.macromol.6b00667

data_1554165
_publ_section_title
;
 Addition-Isomerization Polymerization of Chiral Phosphaalkenes:
 Observation of Styrene--Phosphaalkene Linkages in a Random Copolymer
;
_journal_issue                   11
_journal_name_full               Macromolecules
_journal_page_first              4067
_journal_paper_doi               10.1021/acs.macromol.6b00667
_journal_volume                  49
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C37 H48 N O P'
_chemical_formula_sum            'C37 H48 N O P'
_chemical_formula_weight         553.73
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                94.563(7)
_cell_angle_beta                 96.525(6)
_cell_angle_gamma                114.894(6)
_cell_formula_units_Z            2
_cell_length_a                   10.369(3)
_cell_length_b                   10.511(3)
_cell_length_c                   16.499(4)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.32
_cell_volume                     1604.3(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25215
_diffrn_reflns_point_group_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.461
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0616 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8911.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2644 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         10331
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.7047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1161
_reflns_Friedel_coverage         0.573
_reflns_Friedel_fraction_full    0.584
_reflns_Friedel_fraction_max     0.570
_reflns_number_gt                8339
_reflns_number_total             10331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b00667_si_002.cif
_cod_data_source_block           mo_dg283_0m_b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1604.2(7)
_cod_database_code               1554165
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.982
_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. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C33A)
Uanis(C32) = Uanis(C32A)
Uanis(C31) = Uanis(C31A)
Uanis(C70) = Uanis(C70A)
Uanis(C68) = Uanis(C68A)
Uanis(C69) = Uanis(C69A)
3. Others
 Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=
 Sof(H70F)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(1)
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(2)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(2)
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=1-FVAR(3)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C17(H17), C53(H53), C54(H54)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C52(H52A,H52B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C22(H22), C24(H24), C11(H11), C7(H7), C44(H44), C6(H6), C12(H12),
 C43(H43), C50(H50), C42(H42), C59(H59), C13(H13), C61(H61), C46(H46), C49(H49),
  C3(H3), C48(H48), C40(H40), C4(H4), C41(H41), C5(H5)
4.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C72(H72A,H72B,
 H72C), C74(H74A,H74B,H74C), C36(H36A,H36B,H36C), C64(H64A,H64B,H64C), C37(H37A,
 H37B,H37C), C69(H69A,H69B,H69C), C66(H66A,H66B,H66C), C55(H55A,H55B,H55C),
 C65(H65A,H65B,H65C), C56(H56A,H56B,H56C), C68(H68A,H68B,H68C), C18(H18A,H18B,
 H18C), C31(H31A,H31B,H31C), C19(H19A,H19B,H19C), C73(H73A,H73B,H73C), C35(H35A,
 H35B,H35C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C70(H70A,H70B,H70C),
 C69A(H69D,H69E,H69F), C70A(H70D,H70E,H70F), C68A(H68D,H68E,H68F), C32A(H32D,
 H32E,H32F), C31A(H31D,H31E,H31F), C33A(H33D,H33E,H33F), C36A(H36D,H36E,H36F),
 C35A(H35D,H35E,H35F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'