Dynamic behaviour in nonporous hybrid metal‒organic materials via mechanochemical and gas‒solid reactions
Guo, Fang; Wang, Hao-Cheng; Famulari, Antonino; Lu, Hai-Dong; Martí-Rujas, Javier; CrystEngComm 20 (2018) 6721–; doi:10.1039/C8CE01287C

data_7231597
_publ_section_title
;
 Dynamic behaviour in nonporous hybrid metal--organic materials via
 mechanochemical and gas--solid reactions
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6721
_journal_paper_doi               10.1039/C8CE01287C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C24 H36 Cl4 Cu2 N4, C2 H3 N'
_chemical_formula_sum            'C26 H38 Cl4 Cu2 N5'
_chemical_formula_weight         689.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-29
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-25 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.363(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1550(8)
_cell_length_b                   13.1686(9)
_cell_length_c                   20.0070(13)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.319
_cell_measurement_theta_min      3.127
_cell_volume                     3196.9(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24469
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         3.127
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1167 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.6355.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0684
_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^)+15.7161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5594
_reflns_number_total             7693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01287c2.cif
_cod_data_source_block           1ppMeCN
_cod_depositor_comments
'Adding full bibliography for 7231595--7231597.cif.'
_cod_database_code               7231597
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3), N2(H2), C7(H7), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C18(H18A,H18B), C20(H20A,H20B), C24(H24A,H24B), C8(H8A,H8B),
 C12(H12A,H12B), C21(H21A,H21B), C23(H23A,H23B), C9(H9A,H9B), C22(H22A,H22B),
 C11(H11A,H11B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C13(H13), C4(H4), C2(H2A), C3(H3A), C14(H14), C16(H16), C15(H15)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'