Nickel adipate coordination polymers with isomeric dipyridylamide ligands: topological disorder and divergent magnetic properties
White, Charmaine L.; LaDuca, Robert L.; CrystEngComm 18 (2016) 6789–; doi:10.1039/C6CE01368F

data_7226033
_publ_section_title
;
 Nickel adipate coordination polymers with isomeric dipyridylamide
 ligands: topological disorder and divergent magnetic properties
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              6789
_journal_paper_doi               10.1039/C6CE01368F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C34 H35 N6 Ni2 O11, 2(H2 O)'
_chemical_formula_sum            'C34 H39 N6 Ni2 O13'
_chemical_formula_weight         857.13
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-13 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.375(2)
_cell_angle_beta                 73.490(2)
_cell_angle_gamma                74.612(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2195(18)
_cell_length_b                   13.111(2)
_cell_length_c                   13.874(2)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.79
_cell_volume                     1863.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6898
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.464
_diffrn_reflns_theta_min         1.550
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0674 before and 0.0576 after correction.
 The Ratio of minimum to maximum transmission is 0.70.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0877 before and 0.0699 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 38041 reflections, Rint = 0.0903
 (10538 with I > 3sig(I), Rint = 0.0582)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6898
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4768
_reflns_number_total             6898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01368f2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7226032--7226033.cif.'
_cod_database_code               7226033
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.859
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C12A-C11A
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C11) = Uanis(C9) = Uanis(C8)
Uanis(C9A) = Uanis(C10A) = Uanis(C12A) = Uanis(C11A) = Uanis(C8A) = Uanis(O7A)
= Uanis(O8A)
4. Others
 Fixed Sof: O7(0.75) O8(0.75) C8(0.75) H8A(0.75) H8B(0.75) C9(0.75) H9A(0.75)
 H9B(0.75) C10(0.75) H10A(0.75) H10B(0.75) C11(0.75) H11A(0.75) H11B(0.75)
 C12(0.75) C9A(0.25) H9AA(0.25) H9AB(0.25) C10A(0.25) H10C(0.25) H10D(0.25)
 C12A(0.25) C11A(0.25) H11C(0.25) H11D(0.25) C8A(0.25) H8AA(0.25) H8AB(0.25)
 O7A(0.25) O8A(0.25)
5.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C9A(H9AA,H9AB), C10A(H10C,H10D), C11A(H11C,
 H11D), C8A(H8AA,H8AB)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31),
  C32(H32), C34(H34)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'