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_7229069
_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         'C28 H14 N5 Ni O9, 2(C3 H7 N O)'
_chemical_formula_sum            'C37 H35 N8 Ni O12'
_chemical_formula_weight         842.44
_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
_audit_creation_date             2016-03-10
_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                89.642(4)
_cell_angle_beta                 83.978(5)
_cell_angle_gamma                82.956(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8571(6)
_cell_length_b                   11.2573(7)
_cell_length_c                   16.1205(8)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3240
_cell_measurement_theta_min      3.9680
_cell_volume                     1765.46(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -94.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  150.0000 92

  2 omega  -94.00   -2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -90.0000 92

  3 omega   20.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292   38.0000 -120.0000 95

  4 omega   83.00  123.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 40

  5 omega  -30.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292  -38.0000   60.0000 95

  6 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 61

  7 omega   33.00  122.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   30.0000 89

  8 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   90.0000 61

  9 omega   30.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 61

 10 omega   83.00  176.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 93

 11 omega  151.00  176.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 25

 12 omega  102.00  143.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  120.0000 41

 13 omega   30.00   79.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -150.0000 49

 14 omega  131.00  167.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000    0.0000 36

 15 omega   82.00  114.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000    0.0000 32

 16 omega   36.00  131.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000   30.0000 95

 17 omega   34.00   59.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  120.0000 25

 18 omega   89.00  130.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -180.0000 41

 19 omega   38.00  136.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -150.0000 98

 20 omega   62.00  121.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -150.0000 59
;
_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      0.0318280000
_diffrn_orient_matrix_UB_12      -0.0696314000
_diffrn_orient_matrix_UB_13      -0.0831302000
_diffrn_orient_matrix_UB_21      0.1539489000
_diffrn_orient_matrix_UB_22      0.0116418000
_diffrn_orient_matrix_UB_23      0.0008544000
_diffrn_orient_matrix_UB_31      0.0190318000
_diffrn_orient_matrix_UB_32      -0.1184517000
_diffrn_orient_matrix_UB_33      0.0482020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14637
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.646
_diffrn_reflns_theta_min         3.957
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.927
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.0891
_exptl_crystal_size_mid          0.0612
_exptl_crystal_size_min          0.0362
_refine_diff_density_max         1.918
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0956P)^2^+1.7483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6112
_reflns_number_total             6882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00956a2.cif
_cod_data_source_block           nhbnen_sq
_cod_database_code               7229069
_nottingham_internal_coll_name   NHBNEN
_nottingham_internal_coll_number 15708
_nottingham_internal_coll_client NHB/NRC
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '30.0000, 120.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pczcrp
_nottingham_internal_coll_date   04/03/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 10/03/2016
_nottingham_internal_process_user pczcrp
_nottingham_internal_solution_date 10/03/2016
_nottingham_internal_solution_user pczcrp
_nottingham_internal_refinement_date 10/03/2016
_nottingham_internal_refinement_user pczcrp
_nottingham_internal_self_archive_date 10/03/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C48H24Ni2N2O18
_chemical_oxdiff_usercomment
'#15708 NHBNEN GVB-933 FOMBLIM ON MICROMOUNT FOR NHB/NRC'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C26(H26), C16(H16), C28(H28), C17(H17), C23(H23), C20(H20),
 C4(H4), C21(H21), C2(H2), C24(H24), C12(H12), C11(H11), C32(H32), C29(H29)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              13495
_shelx_fab_checksum              84090
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'