Crystal structure of catena-poly[tetraaqua-bis(μ2-2-(4-carboxylatophenoxy)benzoato-κ2 O:O′)-pentakis(pyridine-κ1 N)dinickel(II)], C53H47N5Ni2O13
Wu, Hao; Zhang, Li; Ma, Yun; Du, Weichao; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 711–713; doi:10.1515/ncrs-2019-0063

data_8105828
_publ_section_title
;
 Crystal structure of
 catena-poly[tetraaqua-bis(\m2-2-(4-carboxylatophenoxy)benzoato-\k2
 O:O&#x2032;)-pentakis(pyridine-\k1 N)dinickel(II)], C53H47N5Ni2O13
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              711
_journal_page_last               713
_journal_paper_doi               10.1515/ncrs-2019-0063
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         '0.5(C106 H94 N10 Ni4 O26)'
_chemical_formula_sum            'C53 H47 N5 Ni2 O13'
_chemical_formula_weight         1079.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 130.953(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0549(15)
_cell_length_b                   14.5539(4)
_cell_length_c                   18.8986(11)
_cell_measurement_reflns_used    2954
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3109
_cell_measurement_theta_min      2.9969
_cell_volume                     4996.9(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -54.00   45.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4204    0.0000 -120.0000 99

  2 omega    6.00   65.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4204 -110.0000   56.0000 59

  3 omega   59.00   84.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4204 -178.0000   30.0000 25

  4 omega  -40.00  -13.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4204  -37.0000 -180.0000 27

  5 omega   14.00   40.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4204  -37.0000 -180.0000 26

  6 omega   -3.00   23.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0454  -99.0000 -150.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0023636000
_diffrn_orient_matrix_UB_12      -0.0473443000
_diffrn_orient_matrix_UB_13      -0.0066395000
_diffrn_orient_matrix_UB_21      -0.0021096000
_diffrn_orient_matrix_UB_22      0.0110279000
_diffrn_orient_matrix_UB_23      -0.0382653000
_diffrn_orient_matrix_UB_31      0.0389098000
_diffrn_orient_matrix_UB_32      0.0034716000
_diffrn_orient_matrix_UB_33      0.0309867000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11813
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+5.0499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3948
_reflns_number_total             5099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0063_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        4996.9(7)
_cod_database_code               8105828
_chemical_oxdiff_formula         'C H O N  Ni'
_chemical_oxdiff_usercomment     ncy-p166
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.827
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H,H) groups
2. Restrained distances
 C19A-C20 = C19A-C18A = C21-C20 = C21A-C20
 1.39 with sigma of 0.01
3. Restrained planarity
 C18, C19, C20, C21, C22
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C18 \\sim C19 \\sim C20 \\sim C21: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(H20)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=1-FVAR(1)
 Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(H20A)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=FVAR(1)
 Fixed Sof: H7A(0.5) H7B(0.5)
6.a Riding coordinates:
 O6(H6A,H6B)
6.b Rotating group:
 O7(H7A,H7B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C18A(H18A), C19(H19), C19A(H19A),
 C20(H20), C20(H20A), C21(H21), C21A(H21A), C22(H22), C22A(H22A), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;