Stereoregular Two-Dimensional Polymers Constructed by Topochemical Polymerization
Wang, Zhihan; Randazzo, Katelyn; Hou, Xiaodong; Simpson, Jeffrey; Struppe, Jochem; Ugrinov, Angel; Kastern, Brent; Wysocki, Erin; Chu, Qianli R.; Macromolecules 48 (2015) 2894–; doi:10.1021/acs.macromol.5b00109

data_1554151
_publ_section_title
;
 Stereoregular Two-Dimensional Polymers Constructed by Topochemical
 Polymerization
;
_journal_issue                   9
_journal_name_full               Macromolecules
_journal_page_first              2894
_journal_paper_doi               10.1021/acs.macromol.5b00109
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         '2(C18 H14 O4), 4(C2 H9 N2), 2(H2 O)'
_chemical_formula_sum            'C44 H68 N8 O10'
_chemical_formula_weight         869.06
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2260(3)
_cell_length_b                   20.5019(8)
_cell_length_c                   24.2730(9)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.688
_cell_measurement_theta_min      2.828
_cell_volume                     4565.0(3)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63605
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.683
_diffrn_reflns_theta_min         2.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1054 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8686.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         8043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1336P)^2^+2.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6544
_reflns_number_total             8043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma5b00109_si_003.cif
_cod_data_source_block           cu_zxw4_0m
_cod_database_code               1554151
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6SC,H6SD} of N6SB, {H44A,H44B} of N44, {H6SA,H6SB} of
  N6SA, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups, All O(H,
  H,H,H) groups
 At 1.5 times of:
  {H1SA,H1SB} of N1S, {H4SA,H4SB} of N4S
2. Others
 Sof(H7SC)=Sof(H7SD)=Sof(N6SB)=Sof(H6SC)=Sof(H6SD)=Sof(C8SB)=Sof(H8SC)=
 Sof(H8SD)=1-FVAR(1)
 Sof(N6SA)=Sof(H6SA)=Sof(H6SB)=Sof(C8SA)=Sof(H8SA)=Sof(H8SB)=Sof(H7SA)=
 Sof(H7SB)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C1S(H1SC,H1SD), C2S(H2SD,H2SE), C4S(H4SC,H4SD), C42(H42A,H42B), C5S(H5SD,
 H5SE), C6S(H6SE,H6SF), C8SA(H8SA,H8SB), C7S(H7SA,H7SB), C7S(H7SC,H7SD),
 C8SB(H8SC,H8SD)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34)
3.d Idealised Me refined as rotating group:
 N2S(H2SA,H2SB,H2SC), N3S(H3SA,H3SB,H3SC), N9(H9A,H9B,H9C), N5S(H5SA,H5SB,H5SC)
;
_shelx_res_checksum              57368
_shelx_hkl_checksum              64674