Crystal structure of hexakis(μ2-azido-κ2N:N)-diazido-κ1N-tetrakis(phenanthroline-κ2N,N′)tetrazinc(II), C48H32N32Zn4
Feng, Yu-Quan; Zhong, Zhi-Guo; Yue, Zi-Long; Zeitschrift für Kristallographie - New Crystal Structures 235 (2019) 57–58; doi:10.1515/ncrs-2019-0473

data_8105015
_publ_section_title
;
 Crystal structure of
 hexakis(\m2-azido-\k2N:N)-diazido-\k1N-tetrakis(phenanthroline-\k2N,N&#x2032;)tetrazinc(II),
 C48H32N32Zn4
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              57
_journal_page_last               58
_journal_paper_doi               10.1515/ncrs-2019-0473
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         'C48 H32 N32 Zn4'
_chemical_formula_sum            'C48 H32 N32 Zn4'
_chemical_formula_weight         1318.59
_chemical_name_systematic
;
tetra-(1,10-phenanthroline-N,N') octa-(azido-N) tetra-zinc(II)
;
_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
_cell_angle_alpha                71.710(2)
_cell_angle_beta                 76.166(2)
_cell_angle_gamma                71.086(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9928(14)
_cell_length_b                   10.1374(14)
_cell_length_c                   14.2362(19)
_cell_measurement_reflns_used    2613
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.20
_cell_volume                     1280.1(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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    'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9865
_diffrn_measured_fraction_theta_max 0.9865
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8227
_diffrn_reflns_theta_full        25.9987
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.6995
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.7103
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             665.3801
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.3660
_refine_diff_density_min         -0.3388
_refine_diff_density_rms         0.0874
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             9.3420
_refine_ls_goodness_of_fit_ref   1.0249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4969
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.0236
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0356P)^2^+0.3082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -11
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3848
_reflns_number_total             4969
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ncrs-2019-0473_suppl.cif
_cod_data_source_block           A
_cod_database_code               8105015
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N14) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'