Coordination polymers from a highly flexible alkyldiamine-derived ligand: structure, magnetism and gas adsorption studies.
Hawes, Chris S.; Chilton, Nicholas F.; Moubaraki, Boujemaa; Knowles, Gregory P.; Chaffee, Alan L.; Murray, Keith S.; Batten, Stuart R.; Turner, David R.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17494–17507; doi:10.1039/c5dt02323h

data_7035864
_publ_section_title
;
 Coordination polymers from a highly flexible alkyldiamine-derived ligand:
 structure, magnetism and gas adsorption studies.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17494
_journal_page_last               17507
_journal_paper_doi               10.1039/c5dt02323h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C42 H52 N2 O12 S4 Zn2'
_chemical_formula_sum            'C42 H52 N2 O12 S4 Zn2'
_chemical_formula_weight         1035.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-14 deposited with the CCDC.
2015-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.437(3)
_cell_length_b                   15.586(3)
_cell_length_c                   30.335(6)
_cell_measurement_reflns_used    7986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.845
_cell_measurement_theta_min      1.469
_cell_volume                     5880(2)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35387
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.800
_diffrn_reflns_theta_max         22.845
_diffrn_reflns_theta_min         1.469
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         7986
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1372P)^2^+10.8942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5655
_reflns_number_total             7986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02323h2.cif
_cod_data_source_block           3
_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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035861--7035865.cif.
;
_cod_database_code               7035864
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All C(H,H,H,H,H,H,H,H,H)
  groups
2. Restrained distances
 S62-C65
 1.75 with sigma of 0.02
 C66-S63
 1.75 with sigma of 0.02
 C64-S63
 1.75 with sigma of 0.02
 S62-C64
 1.75 with sigma of 0.02
 S69-C70
 1.75 with sigma of 0.02
 S68-C70
 1.75 with sigma of 0.02
 S69-C71
 1.75 with sigma of 0.02
 S68-C71
 1.75 with sigma of 0.02
 S56-C57
 1.75 with sigma of 0.02
 S55-C57
 1.75 with sigma of 0.02
 S54-C57
 1.75 with sigma of 0.02
 C58-S56
 1.75 with sigma of 0.02
 S55-C59
 1.75 with sigma of 0.02
 C60-S54
 1.75 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S63, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S62, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: S48(0.5) H49A(0.5) H49B(0.5) H49C(0.5) H49D(0.5) H49E(0.5)
 H49F(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) S51(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) S54(0.33333) S55(0.33333) S56(0.33333) H57G(0.33333)
 H57H(0.33333) H57I(0.33333) H57A(0.33333) H57B(0.33333) H57C(0.33333)
 H57D(0.33333) H57E(0.33333) H57F(0.33333) C58(0.33333) H58A(0.33333)
 H58B(0.33333) H58C(0.33333) C59(0.33333) H59A(0.33333) H59B(0.33333)
 H59C(0.33333) C60(0.33333) H60A(0.33333) H60B(0.33333) H60C(0.33333) S62(0.5)
 S63(0.5) H64D(0.5) H64E(0.5) H64F(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5)
 H65A(0.5) H65B(0.5) H65C(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) S68(0.5)
 S69(0.5) H70A(0.5) H70B(0.5) H70C(0.5) H70D(0.5) H70E(0.5) H70F(0.5) H71A(0.5)
 H71B(0.5) H71C(0.5) H71D(0.5) H71E(0.5) H71F(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C24(H24A,H24B), C34(H34A,H34B), C36(H36A,
 H36B), C46(H46A,H46B)
6.b Me refined with riding coordinates:
 C49(H49A,H49B,H49C), C49(H49D,H49E,H49F), C57(H57G,H57H,H57I), C57(H57A,H57B,
 H57C), C57(H57D,H57E,H57F), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C64(H64D,H64E,H64F), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C),
 C70(H70D,H70E,H70F), C71(H71A,H71B,H71C), C71(H71D,H71E,H71F)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C16(H16), C17(H17), C19(H19), C20(H20),
 C29(H29), C30(H30), C32(H32), C33(H33), C38(H38), C39(H39), C41(H41), C42(H42)
6.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C)
;
_shelx_res_checksum              87515
_shelx_fab_checksum              72788
_olex2_submission_special_instructions 'No special instructions were received'