The enhancement of chain rigidity and gas transport performance of polymers of intrinsic microporosity via intramolecular locking of the spiro-carbon
Jian Zhang; Hong Kang; Jacob Martin; Shouhai Zhang; Sylvie Thomas; Tim C. Merkel; Jianyong Jin; Chem.Commun. 52 (2016) 6553–; doi:

data_7119102
_publ_section_title
;
 The enhancement of chain rigidity and gas transport performance of
 polymers of intrinsic microporosity via intramolecular locking of the
 spiro-carbon
;
_journal_name_full               Chem.Commun.
_journal_page_first              6553
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C47 H82 O5 Si4'
_chemical_formula_sum            'C47 H82 O5 Si4'
_chemical_formula_weight         839.49
_chemical_name_common            'monomer of PIM-C1'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-08-13 deposited with the CCDC.
2016-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                106.876(3)
_cell_angle_beta                 92.299(3)
_cell_angle_gamma                109.501(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8267(6)
_cell_length_b                   13.4665(7)
_cell_length_c                   18.3608(9)
_cell_measurement_temperature    372(2)
_cell_volume                     2607.2(2)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      372(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  BrukerAPEXII
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38723
_diffrn_reflns_theta_full        24.29
_diffrn_reflns_theta_max         24.29
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1095 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.8658.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+1.4481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                5853
_reflns_number_total             8237
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6cc02308h2.cif
_cod_data_source_block           ttsbi_0m
_cod_database_code               7119102
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.036) H6A(0.032) H6B(0.032) H7A(0.033) H7B(0.033) H14(0.03)
 H17A(0.05) H17B(0.05) H17C(0.05) H18A(0.048) H18B(0.048) H18C(0.048)
 H19A(0.031) H19B(0.031) H20A(0.03) H20B(0.03) H22A(0.057) H22B(0.057)
 H22C(0.057) H23A(0.057) H23B(0.057) H23C(0.057) H24A(0.06) H24B(0.06)
 H24C(0.06) H25A(0.067) H25B(0.067) H25C(0.067) H27A(0.083) H27B(0.083)
 H27C(0.083) H28A(0.069) H28B(0.069) H28C(0.069) H29A(0.07) H29B(0.07)
 H29C(0.07) H30A(0.062) H30B(0.062) H30C(0.062) H31A(0.058) H31B(0.058)
 H31C(0.058) H33A(0.091) H33B(0.091) H33C(0.091) H34A(0.079) H34B(0.079)
 H34C(0.079) H35A(0.072) H35B(0.072) H35C(0.072) H36A(0.08) H36B(0.08)
 H36C(0.08) H37A(0.118) H37B(0.118) H37C(0.118) H39A(0.103) H39B(0.103)
 H39C(0.103) H40A(0.115) H40B(0.115) H40C(0.115) H41A(0.146) H41B(0.146)
 H41C(0.146) H42A(0.065) H42B(0.065) H42C(0.065) H43A(0.053) H43B(0.053)
 H43C(0.053) H45A(0.094) H45B(0.094) H45C(0.094) H46A(0.083) H46B(0.083)
 H46C(0.083) H47A(0.09) H47B(0.09) H47C(0.09)
 Fixed X: H2(0.7716) H6A(0.4937) H6B(0.6051) H7A(0.5084) H7B(0.6003)
 H14(0.8642) H17A(0.9692) H17B(1.006) H17C(0.8687) H18A(1.062) H18B(1.1267)
 H18C(1.0808) H19A(0.8566) H19B(0.9711) H20A(0.853) H20B(0.973) H22A(1.0193)
 H22B(1.0847) H22C(1.0113) H23A(0.896) H23B(0.9601) H23C(0.8182) H24A(0.4563)
 H24B(0.5334) H24C(0.4581) H25A(0.7032) H25B(0.7569) H25C(0.8157) H27A(0.8208)
 H27B(0.6984) H27C(0.8064) H28A(0.6785) H28B(0.5668) H28C(0.6013) H29A(0.8069)
 H29B(0.8866) H29C(0.8679) H30A(0.3732) H30B(0.2377) H30C(0.3428) H31A(0.2494)
 H31B(0.1729) H31C(0.302) H33A(0.2451) H33B(0.3517) H33C(0.2202) H34A(0.3661)
 H34B(0.2584) H34C(0.2397) H35A(0.0621) H35B(0.0849) H35C(0.0756) H36A(0.3839)
 H36B(0.3195) H36C(0.4615) H37A(0.4623) H37B(0.3206) H37C(0.4021) H39A(0.2087)
 H39B(0.3012) H39C(0.1651) H40A(0.0794) H40B(0.1621) H40C(0.1338) H41A(0.2238)
 H41B(0.3615) H41C(0.3079) H42A(0.5829) H42B(0.7041) H42C(0.6531) H43A(0.9059)
 H43B(0.9447) H43C(0.9527) H45A(0.5727) H45B(0.5827) H45C(0.6223) H46A(0.8087)
 H46B(0.887) H46C(0.758) H47A(0.7908) H47B(0.9073) H47C(0.8296)
 Fixed Y: H2(-0.2261) H6A(0.0515) H6B(0.1339) H7A(0.0058) H7B(-0.025)
 H14(0.4387) H17A(0.4756) H17B(0.4141) H17C(0.392) H18A(0.2846) H18B(0.3526)
 H18C(0.4111) H19A(0.2046) H19B(0.1828) H20A(0.0304) H20B(0.1081) H22A(0.0396)
 H22B(0.0039) H22C(-0.0842) H23A(-0.2038) H23B(-0.1167) H23C(-0.1634) H24A(-
 0.4261) H24B(-0.5028) H24C(-0.4999) H25A(-0.4444) H25B(-0.4531) H25C(-0.3457)
 H27A(-0.3279) H27B(-0.3547) H27C(-0.2423) H28A(-0.1373) H28B(-0.2468) H28C(-
 0.1494) H29A(-0.103) H29B(-0.1741) H29C(-0.0936) H30A(-0.3492) H30B(-0.4031)
 H30C(-0.3953) H31A(-0.0907) H31B(-0.2109) H31C(-0.1471) H33A(-0.0679) H33B(-
 0.0789) H33C(-0.1179) H34A(-0.2672) H34B(-0.3739) H34C(-0.3006) H35A(-0.292)
 H35B(-0.3571) H35C(-0.2399) H36A(0.1733) H36B(0.2592) H36C(0.3002)
 H37A(0.4125) H37B(0.3618) H37C(0.3416) H39A(0.0248) H39B(-0.0177) H39C(-
 0.0602) H40A(0.0665) H40B(0.1853) H40C(0.163) H41A(-0.004) H41B(0.0391)
 H41C(0.1181) H42A(0.5153) H42B(0.6116) H42C(0.604) H43A(0.6092) H43B(0.6092)
 H43C(0.5171) H45A(0.3386) H45B(0.2535) H45C(0.2455) H46A(0.3909) H46B(0.4908)
 H46C(0.4831) H47A(0.2583) H47B(0.3528) H47C(0.2574)
 Fixed Z: H2(0.2831) H6A(0.3463) H6B(0.3241) H7A(0.1246) H7B(0.1695)
 H14(0.2519) H17A(0.3856) H17B(0.4377) H17C(0.4142) H18A(0.2511) H18B(0.3359)
 H18C(0.2851) H19A(0.3863) H19B(0.355) H20A(0.161) H20B(0.2187) H22A(0.3365)
 H22B(0.2663) H22C(0.3036) H23A(0.1767) H23B(0.1363) H23C(0.1289) H24A(0.4398)
 H24B(0.4276) H24C(0.3566) H25A(0.2915) H25B(0.3679) H25C(0.345) H27A(0.5155)
 H27B(0.549) H27C(0.5899) H28A(0.5862) H28B(0.5457) H28C(0.5106) H29A(0.4541)
 H29B(0.4589) H29C(0.5344) H30A(0.2239) H30B(0.2341) H30C(0.2928) H31A(0.2923)
 H31B(0.2373) H31C(0.2215) H33A(0.4365) H33B(0.4833) H33C(0.504) H34A(0.4635)
 H34B(0.4131) H34C(0.4919) H35A(0.4226) H35B(0.3422) H35C(0.3559) H36A(0.2569)
 H36B(0.2619) H36C(0.277) H37A(0.156) H37B(0.1346) H37C(0.0708) H39A(0.1641)
 H39B(0.1178) H39C(0.0805) H40A(0.0492) H40B(0.05) H40C(0.1277) H41A(-0.0318)
 H41B(0.0023) H41C(-0.0227) H42A(0.0603) H42B(0.0629) H42C(0.1394) H43A(0.1976)
 H43B(0.1169) H43C(0.1509) H45A(-0.0422) H45B(-0.0018) H45C(-0.0831) H46A(-
 0.098) H46B(-0.0259) H46C(-0.0571) H47A(0.043) H47B(0.0368) H47C(-0.0378)
;