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_7229068
_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_absolute_configuration ad
_chemical_formula_moiety         'C30 H26 N8 Ni O12'
_chemical_formula_sum            'C90 H174 N28 Ni O36'
_chemical_formula_weight         2283.27
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-15 deposited with the CCDC.
2017-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5137(6)
_cell_length_b                   19.5137(6)
_cell_length_c                   22.1533(16)
_cell_measurement_reflns_used    5227
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1190
_cell_measurement_theta_min      5.1250
_cell_volume                     8435.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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_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 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      6.00  35.00   1.00   20.00    --  -38.50  77.00 -60.00   29
  2  \w    -70.00  17.00   1.00   20.00    --  -38.50  77.00 150.00   87
  3  \w     73.00 172.00   1.00   80.00    --  104.50  77.00-180.00   99
  4  \w     81.00 163.00   1.00   80.00    --  104.50  77.00 150.00   82
  5  \w    136.00 163.00   1.00   80.00    --  104.50  77.00 -90.00   27
  6  \w     83.00 126.00   1.00   80.00    --  104.50  77.00 -90.00   43
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0395204000
_diffrn_orient_matrix_UB_12      -0.0526642000
_diffrn_orient_matrix_UB_13      0.0385825000
_diffrn_orient_matrix_UB_21      -0.0048600000
_diffrn_orient_matrix_UB_22      -0.0479910000
_diffrn_orient_matrix_UB_23      -0.0548759000
_diffrn_orient_matrix_UB_31      0.0681818000
_diffrn_orient_matrix_UB_32      -0.0338903000
_diffrn_orient_matrix_UB_33      0.0184559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9272
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.397
_diffrn_reflns_theta_min         4.532
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent diffraction microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.596
_exptl_crystal_description       block
_exptl_crystal_F_000             9808
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     489
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1119P)^2^+23.4050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                3408
_reflns_number_total             3635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00956a2.cif
_cod_data_source_block           nhbnfr_sq
_cod_original_cell_volume        8435.7(8)
_cod_database_code               7229068
_nottingham_internal_coll_name   NHBNFR
_nottingham_internal_coll_number 16240
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 20.00, 80.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_coll_date   18/06/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 19/06/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 19/06/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 19/06/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 19/06/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C48H24O12N4Ni2
_chemical_oxdiff_usercomment
'NHBNFR 16240 GVB-1074 IN FOMBLIN FILM ON MICROMOUNT FOR CRP/NRC'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(9) 0.17(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N6A)=1-FVAR(1)
 Sof(O4)=Sof(O5)=Sof(O6)=Sof(N6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15)
6.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              25311
_shelx_fab_checksum              82600
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.486
_oxdiff_exptl_absorpt_empirical_full_min 0.394