Structural chemistry and selective CO2uptake of a piperazine-derived porous coordination polymer
Hawes, Chris S.; White, Keith F.; Abrahams, Brendan F.; Knowles, Gregory P.; Chaffee, Alan L.; Batten, Stuart R.; Turner, David R.; CrystEngComm 17 (2015) 2196–; doi:10.1039/C4CE02547D

data_7219374
_publ_section_title
;
 Structural chemistry and selective CO2uptake of a piperazine-derived
 porous coordination polymer
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2196
_journal_paper_doi               10.1039/C4CE02547D
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C40 H42 N4 O10 Zn3, C6 H14 N2 O2'
_chemical_formula_sum            'C46 H56 N6 O12 Zn3'
_chemical_formula_weight         1081.08
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
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2014-12-22 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.76(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.666(7)
_cell_length_b                   24.302(6)
_cell_length_c                   6.0130(12)
_cell_measurement_reflns_used    13301
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.88
_cell_measurement_theta_min      2.88
_cell_volume                     2536.1(13)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71090
_diffrn_reflns_av_R_equivalents  0.1644
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23326
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.674
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                2682
_reflns_number_total             3438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02547d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7219372--7219374.cif.
;
_cod_database_code               7219374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H12A of C12A, H9 of C9, H18 of C18, H8 of C8, H11A of
  C11A, H8A of C8A, H11 of C11, H9A of C9A, H12 of C12
 At 1.5 times of:
  All C(H,H,H) groups, H3 of C9
2. Restrained distances
 O3-H3
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O4(0.5) C9A(0.5) H9A(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5)
 C8A(0.5) H8A(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) O4A(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C12A(0.5) H12A(0.5) C11A(0.5) H11A(0.5) C8(0.5)
 H8(0.5) C9(0.5) H9(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C11(H11), C12(H12), C8A(H8A), C18(H18), C12A(H12A), C11A(H11A),
 C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'