Crystal Melting and Glass Formation in Copper Thiocyanate based Coordination Polymers
Nagarkar, Sanjog S.; Kurasho, Haruna; Duong, Nghia Tuan Tuan; Nishiyama, Yusuke; Kitagawa, Susumu; Horike, Satoshi; Chemical Communications  (2019) –; doi:10.1039/C9CC02172H

data_7123291
_publ_section_title
;
 Crystal Melting and Glass Formation in Copper Thiocyanate based
 Coordination Polymers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02172H
_journal_year                    2019
_chemical_formula_moiety         'C76 H52 Cu8 N20 S12'
_chemical_formula_sum            'C76 H52 Cu8 N20 S12'
_chemical_formula_weight         2138.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2ya'
_space_group_name_H-M_alt        'P 1 a 1'
_symmetry_space_group_name_Hall  'P -2ya'
_symmetry_space_group_name_H-M   'P 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-26 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.097(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.081(6)
_cell_length_b                   19.687(9)
_cell_length_c                   17.017(8)
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.3574
_cell_volume                     4115(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.35
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32165
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.104
_exptl_absorpt_coefficient_mu    2.387
_exptl_absorpt_correction_T_max  0.6467
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         17441
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.1046
_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^)+(0.1064P)^2^+54.8749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2660
_refine_ls_wR_factor_ref         0.2816
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                13768
_reflns_number_total             17441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02172h2.cif
_cod_data_source_block           3_Ph
_cod_original_cell_volume        4116(3)
_cod_database_code               7123291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.647
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C31(H31), C33(H33), C34(H34),
 C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C47(H47), C50(H50), C52(H52), C53(H53), C54(H54), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C67(H67), C68(H68),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C75(H75)
;
_shelx_res_checksum              83185
_olex2_submission_special_instructions 'No special instructions were received'