High Pressure Synthesis of All-Transoid Polycarbonyl [—(C═O)—]n in a Zeolite
Santoro, Mario; Dziubek, Kamil; Scelta, Demetrio; Ceppatelli, Matteo; Gorelli, Federico A.; Bini, Roberto; Thibaud, Jean-Marc; Di Renzo, Francesco; Cambon, Olivier; Rouquette, Jerome; Hermet, Patrick; van der Lee, Arie; Haines, Julien; Chemistry of Materials 27 (2015) 6486–; doi:10.1021/acs.chemmater.5b02596

data_4003186
_publ_section_title
;
 High Pressure Synthesis of All-Transoid Polycarbonyl
 [---(C&#x2550;O)---]n in a Zeolite
;
_journal_issue                   19
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6486
_journal_paper_doi               10.1021/acs.chemmater.5b02596
_journal_volume                  27
_journal_year                    2015
_chemical_formula_sum            'C0.71 O2 Si'
_chemical_formula_weight         68.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            96
_cell_length_a                   19.9880(10)
_cell_length_b                   19.9880(10)
_cell_length_c                   13.3947(9)
_cell_measurement_temperature    293(2)
_cell_volume                     5351.5(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0143
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2915
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        36.356
_diffrn_reflns_theta_max         36.356
_diffrn_reflns_theta_min         3.127
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.533
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_description       prism
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.0797
_exptl_crystal_size_mid          0.0377
_exptl_crystal_size_min          0.0356
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         1263
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0918
_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^)+(0.1534P)^2^+53.1964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1025
_reflns_number_total             1263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm5b02596_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4003186
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              32775
_shelx_hkl_checksum              20106