Trinuclear Ni(ii) oriented highly dense packing and π-conjugation degree of metal‒organic frameworks for efficient water oxidation
Zhai, Zhi-Min; Yang, Xiao-Gang; Yang, Zhao-Tong; Lu, Xiao-Min; Ma, Lu-Fang; CrystEngComm 21 (2019) 5862–; doi:10.1039/C9CE00944B

data_7233613
_publ_section_title
;
 Trinuclear Ni(ii) oriented highly dense packing and \p-conjugation degree
 of metal--organic frameworks for efficient water oxidation
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5862
_journal_paper_doi               10.1039/C9CE00944B
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '2(C9 H11 Ni1.5 O10)'
_chemical_formula_sum            'C18 H22 Ni3 O20'
_chemical_formula_weight         734.44
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-18 deposited with the CCDC.    2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                75.763(5)
_cell_angle_beta                 68.657(5)
_cell_angle_gamma                65.460(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0281(6)
_cell_length_b                   10.0845(5)
_cell_length_c                   13.1425(7)
_cell_measurement_reflns_used    4299
_cell_measurement_temperature    290
_cell_measurement_theta_max      28.0620
_cell_measurement_theta_min      4.0580
_cell_volume                     1119.04(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      290
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_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    -80.00  13.00   1.00    1.79    --  -13.96 -77.00  30.00   93
  2  \w    -41.00  52.00   1.00    1.79    --  -13.96  77.00 150.00   93
  3  \w    -19.00  20.00   1.00    1.79    --  -13.96 -99.00 -90.00   39
  4  \w     46.00  72.00   1.00    1.79    --   14.89  38.00 -30.00   26
  5  \w    -51.00  23.00   1.00    1.79    --   14.89 -77.00 -90.00   74
  6  \w     30.00  55.00   1.00    1.79    --   14.89  57.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399813000
_diffrn_orient_matrix_UB_12      -0.0097859000
_diffrn_orient_matrix_UB_13      -0.0306750000
_diffrn_orient_matrix_UB_21      0.0691282000
_diffrn_orient_matrix_UB_22      -0.0216854000
_diffrn_orient_matrix_UB_23      -0.0435808000
_diffrn_orient_matrix_UB_31      0.0159109000
_diffrn_orient_matrix_UB_32      -0.0740815000
_diffrn_orient_matrix_UB_33      0.0236597000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7822
_diffrn_reflns_theta_full        25.3486
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.1795
_exptl_crystal_description       block
_exptl_crystal_F_000             750.6310
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.7547
_refine_diff_density_min         -1.8878
_refine_diff_density_rms         0.2515
_refine_ls_d_res_high            0.8301
_refine_ls_d_res_low             6.2572
_refine_ls_goodness_of_fit_ref   1.0490
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0490
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.4474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1451
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -11
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3464
_reflns_number_total             4080
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9ce00944b2.cif
_cod_data_source_block           Ni-BTC
_cod_depositor_comments          'Adding full bibliography for 7233613.cif.'
_cod_database_code               7233613
_chemical_oxdiff_formula         C1O1H1N1Ni1
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O14(H14a,H14b), O15(H15a,H15b), O16(H16a,H16b), O18(H18a,H18b), O19(H19a,
 H19b), O20(H20a,H20b)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C11(H11), C13(H13), C15(H15)
;
_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 1.916
_oxdiff_exptl_absorpt_empirical_full_min 0.734