Supramolecular assemblies of new pseudohalide end-to-end bridged copper(II) complex and molecular structural variety of penta and hexa-coordinted metal(II) complexes with hydrazido-based ligand
Singh, Yogendra; Patel, R.N.; Patel, S.K.; Jadeja, R.N.; Patel, A.K.; Patel, N.; Roy, H.; Bhagriya, P.; Singh, Rita; Butcher, R.J.; Jasinski, Jerry P.; Herrero, S.; Cortijo, M.; Inorganica Chimica Acta 503 (2020) 119371–; doi:10.1016/j.ica.2019.119371

data_1565300
_publ_section_title
;
 Supramolecular assemblies of new pseudohalide end-to-end bridged
 copper(II) complex and molecular structural variety of penta and
 hexa-coordinted metal(II) complexes with hydrazido-based ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119371
_journal_paper_doi               10.1016/j.ica.2019.119371
_journal_volume                  503
_journal_year                    2020
_chemical_formula_moiety         'C14 H15 N4 Ni O5, N O3'
_chemical_formula_sum            'C14 H15 N5 Ni O8'
_chemical_formula_weight         440.00
_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                82.246(6)
_cell_angle_beta                 76.509(6)
_cell_angle_gamma                81.090(5)
_cell_formula_units_Z            2
_cell_length_a                   7.2740(5)
_cell_length_b                   8.5854(5)
_cell_length_c                   14.5486(11)
_cell_volume                     868.20(11)
_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)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9760
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5727
_diffrn_reflns_theta_full        67.5000
_diffrn_reflns_theta_max         71.50
_diffrn_reflns_theta_min         5.24
_exptl_absorpt_coefficient_mu    2.148
_exptl_crystal_density_diffrn    1.6829
_exptl_crystal_F_000             447.6409
_refine_diff_density_max         2.4519
_refine_diff_density_min         -1.5559
_refine_diff_density_rms         0.1330
_refine_ls_d_res_high            0.8129
_refine_ls_d_res_low             8.4368
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   2.1932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    26
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      2.1921
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.7321
_refine_ls_shift/su_mean         0.0438
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.7034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1881
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3071
_reflns_number_total             3299
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            YS100Comp.1.cif
_cod_data_source_block           ys-100
_cod_database_code               1565300
_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. Restrained distances
 O1W-H1Wa = O1W-H1Wb
 0.82 with sigma of 0.02
 H1Wa-H1Wb
 1.297 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O21A) = Uiso(O21B)
Uiso(O22A) = Uiso(O22B)
Uiso(O23A) = Uiso(O23B)
4. Same fragment restrains
{O11, O12, O13} sigma for 1-2: 0.02, 1-3: 0.04
as
{O21A, O22A, O23A}
{O11, O12, O13} sigma for 1-2: 0.02, 1-3: 0.04
as
{O21B, O22B, O23B}
5. Others
 Sof(O21B)=Sof(O22B)=Sof(O23B)=1-FVAR(1)
 Sof(O21A)=Sof(O22A)=Sof(O23A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3a), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
6.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'