Crystal structure of (μ2-2,2′-bipyridine-3,3′-dicarboxylato)-bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)-di-nickel(II) perchlorate N,N′-dimethylformamide solvate, C50H92Cl2N12Ni2O14
Li, Huan-Yong; Lin, Wang; Han, Feng-Xian; Ou, Guang-Chuan; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 379–381; doi:10.1515/ncrs-2017-0269

data_8106159
_publ_section_title
;
 Crystal structure of
 (\m2-2,2&#x2032;-bipyridine-3,3&#x2032;-dicarboxylato)-bis(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)-di-nickel(II)
 perchlorate N,N&#x2032;-dimethylformamide solvate, C50H92Cl2N12Ni2O14
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              379
_journal_page_last               381
_journal_paper_doi               10.1515/ncrs-2017-0269
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C44 H78 N10 Ni2 O4, 2(C3 H7 N O), 2(Cl O4)'
_chemical_formula_sum            'C50 H92 Cl2 N12 Ni2 O14'
_chemical_formula_weight         1273.65
_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'
_symmetry_Int_Tables_number      15
_cell_angle_alpha                90
_cell_angle_beta                 114.825(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.731(5)
_cell_length_b                   9.940(2)
_cell_length_c                   26.574(5)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.23
_cell_volume                     6169(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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      173.15
_diffrn_measured_fraction_theta_full 0.9683
_diffrn_measured_fraction_theta_max 0.9683
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14245
_diffrn_reflns_theta_full        27.0539
_diffrn_reflns_theta_max         27.05
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_correction_T_min  0.653201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0723 before and 0.0346 after correction.
The Ratio of minimum to maximum transmission is 0.6532.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.3713
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2717.1549
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.2107
_refine_diff_density_min         -1.3593
_refine_diff_density_rms         0.1558
_refine_ls_d_res_high            0.7813
_refine_ls_d_res_low             11.0112
_refine_ls_goodness_of_fit_ref   1.0487
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    74
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6563
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.0470
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1239P)^2^+11.2645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2209
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              27
_reflns_limit_h_min              -32
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                4169
_reflns_number_total             6563
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2017-0269_suppl.cif
_cod_data_source_block           L
_cod_database_code               8106159
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl1, Cl1a}
3. Restrained distances
 Cl1-O4 = Cl1-O5 = Cl1-O6 = Cl1-O7
 1.44 with sigma of 0.01
 O4-O5 = O4-O6 = O4-O7 = O5-O6 = O5-O7 = O6-O7
 2.35 with sigma of 0.02
 Cl1a-O4a = Cl1a-O5a = Cl1a-O6a = Cl1a-O7a
 1.44 with sigma of 0.01
 O4a-O5a = O4a-O6a = O4a-O7a = O5a-O6a = O5a-O7a = O6a-O7a
 2.35 with sigma of 0.02
4. Rigid bond restraints
 O4, O5, O6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4a, O5a, O6a, O7a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, Cl1a
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O6 \\sim O7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O4a \\sim O5a \\sim O6a \\sim O7a: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl1 \\sim Cl1a: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O4) = Uanis(O4a) = Uanis(O5) = Uanis(O5a) = Uanis(O6) = Uanis(O6a) =
Uanis(O7) = Uanis(O7a)
Uanis(Cl1) = Uanis(Cl1a)
6. Others
 Sof(Cl1a)=Sof(O7a)=Sof(O5a)=Sof(O6a)=Sof(O4a)=1-FVAR(1)
 Sof(O6)=Sof(O5)=Sof(O7)=Sof(O4)=Sof(Cl1)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N1(H1), N4(H4), C15(H15), C7(H7)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C1(H1a,H1b), C14(H14a,H14b), C10(H10a,H10b), C6(H6a,H6b), C9(H9a,
 H9b)
7.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C19(H19), C20(H20), C25(H25)
7.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C8(H8a,H8b,H8c),
 C13(H13a,H13b,H13c), C16(H16a,H16b,H16c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c)
;
_olex2_submission_special_instructions 'No special instructions were received'