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_7035862
_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         'C68 H66 N4 Ni3 O20, 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C74 H84 N6 Ni3 O24'
_chemical_formula_weight         1617.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-02-06
_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                76.18(3)
_cell_angle_beta                 79.76(3)
_cell_angle_gamma                75.16(3)
_cell_formula_units_Z            1
_cell_length_a                   11.878(2)
_cell_length_b                   11.944(2)
_cell_length_c                   13.199(3)
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      1.79
_cell_volume                     1744.1(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Synchrotron
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58284
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0530P)^2^+1.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7763
_reflns_number_total             8335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02323h2.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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7035861--7035865.cif.
;
_cod_database_code               7035862
_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
2. Restrained distances
 N13-H13
 0.88 with sigma of 0.02
 O49-H49A = O49-H49B
 0.84 with sigma of 0.02
 H47A-O47
 0.84 with sigma of 0.02
 O47-H47B
 0.84 with sigma of 0.02
 H48A-O48
 0.84 with sigma of 0.02
 O48-H48B
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C27(H27A,H27B), C37(H37A,H37B), C25(H25A,
 H25B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C30(H30), C11(H11), C19(H19), C33(H33), C43(H43), C8(H8), C10(H10),
 C40(H40), C17(H17), C20(H20), C32(H32), C42(H42), C51(H51), C39(H39), C16(H16),
  C29(H29)
3.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              58665
_olex2_submission_special_instructions 'No special instructions were received'