Nickel(ii) metal‒organic frameworks with N,N′-di(4-pyridyl)-naphthalenediimide ligands: influence of secondary building unit geometry on dimensionality and framework dimensions
Pfeiffer, Constance R.; Biggins, Naomi; Lewis, William; Champness, Neil R.; CrystEngComm  (2017) –; doi:10.1039/C7CE00956A

data_7229067
_publ_section_title
;
 Nickel(ii) metal--organic frameworks with
 N,N&#x2032;-di(4-pyridyl)-naphthalenediimide ligands: influence of
 secondary building unit geometry on dimensionality and framework
 dimensions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00956A
_journal_year                    2017
_chemical_formula_moiety         'C30 H15 N5 Ni O9'
_chemical_formula_sum            'C48 H57 N11 Ni O15'
_chemical_formula_weight         1086.75
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-07-15 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                85.612(3)
_cell_angle_beta                 89.685(3)
_cell_angle_gamma                64.385(6)
_cell_formula_units_Z            2
_cell_length_a                   11.1115(7)
_cell_length_b                   12.5077(8)
_cell_length_c                   16.1965(4)
_cell_measurement_reflns_used    4146
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3830
_cell_measurement_theta_min      4.4180
_cell_volume                     2022.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega   19.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292   57.0000  -90.0000 92

  2 omega  132.00  166.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   30.0000 34

  3 omega  108.00  136.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -60.0000 28

  4 omega   64.00  121.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -180.0000 57

  5 omega   64.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -180.0000 44

  6 omega   45.00  108.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -90.0000 63

  7 omega   35.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000    0.0000 74

  8 omega   89.00  117.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  150.0000 28

  9 omega   59.00  126.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   30.0000 67

 10 omega   97.00  159.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000  -90.0000 62

 11 omega  101.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -150.0000 73

 12 omega   41.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 45

 13 omega   30.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -30.0000 60

 14 omega   41.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -60.0000 28

 15 omega   31.00   66.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -120.0000 35

 16 omega   33.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -180.0000 39

 17 omega  -69.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   77.0000   30.0000 92

 18 omega   34.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 56

 19 omega   31.00   72.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  150.0000 41

 20 omega  -27.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292  -57.0000  120.0000 95

 21 omega    8.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.1131412000
_diffrn_orient_matrix_UB_12      -0.0207722000
_diffrn_orient_matrix_UB_13      0.0427846000
_diffrn_orient_matrix_UB_21      0.0584979000
_diffrn_orient_matrix_UB_22      -0.1270898000
_diffrn_orient_matrix_UB_23      -0.0282580000
_diffrn_orient_matrix_UB_31      0.0862437000
_diffrn_orient_matrix_UB_32      -0.0469274000
_diffrn_orient_matrix_UB_33      0.0805084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14755
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.645
_diffrn_reflns_theta_min         3.933
_diffrn_source                   'microfocus tube'
_diffrn_source_type              'ROD microfocus tube'
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.1555
_exptl_crystal_size_mid          0.0593
_exptl_crystal_size_min          0.0264
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0716P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5761
_reflns_number_total             7891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00956a2.cif
_cod_data_source_block           nhbndn_sq
_cod_original_cell_volume        2022.9(2)
_cod_database_code               7229067
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_date   11/02/2016
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '10.0000, 40.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_name   NHBNDN
_nottingham_internal_coll_number 15629
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_process_date 12/02/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_refinement_date 12/02/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 12/02/2016
_nottingham_internal_solution_date 12/02/2016
_nottingham_internal_solution_user pczcrp
_chemical_oxdiff_formula         C48H24Ni2N2O18
_chemical_oxdiff_usercomment
'NHBNDN #15629 GVB-894 in fomblin on micromount for NHB/NRC'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C014(H014), C015(H015), C016(H016),
 C017(H017), C018(H018), C019(H019)
;
_shelx_res_checksum              81672
_shelx_fab_checksum              83170
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'