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_7226032
_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 H38 N6 Ni2 O12'
_chemical_formula_sum            'C34 H38 N6 Ni2 O12'
_chemical_formula_weight         840.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-09-16
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.16 svn.r3215 for OlexSys, GUI svn.r5095)
;
_audit_update_record
;
2016-06-13 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.2658(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9466(17)
_cell_length_b                   9.4061(7)
_cell_length_c                   20.0971(15)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.28
_cell_volume                     3687.7(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_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(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0587 before and 0.0439 after correction. The Ratio of minimum to maximum transmission is 0.8936. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.144
_refine_diff_density_max         2.062
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     884
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0954P)^2^+11.5351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4920
_reflns_number_total             6771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01368f2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7226032--7226033.cif.'
_cod_database_code               7226032
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.803
_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 O(H,H) groups
2. Restrained distances
 C28-O2
 1.225 with sigma of 0.008
 C28A-O2A
 1.225 with sigma of 0.008
 C17A-O3A
 1.225 with sigma of 0.008
 C17-O3
 1.225 with sigma of 0.008
 C17-N5
 1.348 with sigma of 0.008
 C17A-N5A
 1.348 with sigma of 0.008
 C28A-N2A
 1.348 with sigma of 0.008
 C28-N2
 1.348 with sigma of 0.008
3. Restrained planarity
 N4A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C40B \\sim C41B
\\sim C42B \\sim C43B \\sim C44B \\sim C45B \\sim C40C \\sim C41C \\sim C42C
\\sim C43C \\sim C44C \\sim C45C \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C23A
\\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A
\\sim C31A \\sim C32A \\sim C33A \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C12A
\\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A
\\sim C20A \\sim C21A \\sim C22A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004
N1 \\sim N2 \\sim N3 \\sim N1A \\sim N2A \\sim N3A \\sim N4 \\sim N5 \\sim N6
\\sim N4A \\sim N5A \\sim N6A: within 2A with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(N3) = Uanis(N6)
Uanis(N3A) = Uanis(N6A)
Uanis(O3) = Uanis(O3A)
Uanis(C17) = Uanis(C17A)
Uanis(N4) = Uanis(N1)
Uanis(N1A) = Uanis(N4A)
Uanis(O8B) = Uanis(O11C)
Uanis(O11B) = Uanis(O10C)
5. Same fragment restrains
{O40, O41, O42, O43, C40, C41, C42, C43, C44, C45} sigma for 1-2: 0.02, 1-3:
0.04
as
{O8B, O9B, O10B, O11B, C40B, C41B, C42B, C43B, C44B, C45B}
{O40, O41, O42, O43, C40, C41, C42, C43, C44, C45} sigma for 1-2: 0.02, 1-3:
0.04
as
{O11C, O8C, O9C, O10C, C40C, C41C, C42C, C43C, C44C, C45C}
6. Others
 Fixed Sof: O8B(0.5) O9B(0.5) O10B(0.5) O11B(0.5) C40B(0.5) C41B(0.5)
 H41C(0.5) H41D(0.5) C42B(0.5) H42C(0.5) H42D(0.5) C43B(0.5) H43C(0.5)
 H43D(0.5) C44B(0.5) H44C(0.5) H44D(0.5) C45B(0.5) O11C(0.5) O8C(0.5)
 O9C(0.5) O10C(0.5) C40C(0.5) C41C(0.5) H41E(0.5) H41F(0.5) C42C(0.5)
 H42E(0.5) H42F(0.5) C43C(0.5) H43E(0.5) H43F(0.5) C44C(0.5) H44E(0.5)
 H44F(0.5) C45C(0.5) O2(0.5) N1(0.5) N2(0.5) H2(0.5) N3(0.5) C23(0.5) H23(0.5)
 C24(0.5) H24(0.5) C25(0.5) H25(0.5) C26(0.5) C27(0.5) H27(0.5) C28(0.5)
 C29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33(0.5) O2A(0.5) N1A(0.5) N2A(0.5) H2A(0.5) N3A(0.5) C23A(0.5) H23A(0.5)
 C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5) C26A(0.5) C27A(0.5) H27A(0.5)
 C28A(0.5) C29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5) H31A(0.5) C32A(0.5)
 H32A(0.5) C33A(0.5) H33A(0.5) O3(0.75) N4(0.75) N5(0.75) H5(0.75) N6(0.75)
 C12(0.75) H12(0.75) C13(0.75) H13(0.75) C14(0.75) H14(0.75) C15(0.75)
 C16(0.75) H16(0.75) C17(0.75) C18(0.75) C19(0.75) H19(0.75) C20(0.75)
 H20(0.75) C21(0.75) H21(0.75) C22(0.75) H22(0.75) O3A(0.25) N4A(0.25)
 N5A(0.25) H5A(0.25) N6A(0.25) C12A(0.25) H12A(0.25) C13A(0.25) H13A(0.25)
 C14A(0.25) H14A(0.25) C15A(0.25) C16A(0.25) H16A(0.25) C17A(0.25) C18A(0.25)
 C19A(0.25) H19A(0.25) C20A(0.25) H20A(0.25) C21A(0.25) H21A(0.25) C22A(0.25)
 H22A(0.25) O1WA(0.5) H1WA(0.5) H1WB(0.5) O1WB(0.5) H1WC(0.5) H1WD(0.5)
7.a Free rotating group:
 O1WA(H1WA,H1WB), O1WB(H1WC,H1WD)
7.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C41B(H41C,
 H41D), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,H44D), C41C(H41E,H41F),
 C42C(H42E,H42F), C43C(H43E,H43F), C44C(H44E,H44F)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C23(H23), C24(H24), C25(H25), C27(H27), C30(H30), C31(H31), C32(H32),
 C33(H33), N2A(H2A), C23A(H23A), C24A(H24A), C25A(H25A), C27A(H27A), C30A(H30A),
  C31A(H31A), C32A(H32A), C33A(H33A), N5(H5), C12(H12), C13(H13), C14(H14),
 C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), N5A(H5A), C12A(H12A),
 C13A(H13A), C14A(H14A), C16A(H16A), C19A(H19A), C20A(H20A), C21A(H21A),
 C22A(H22A)
;
_contact_crystallographer_email  staples@chemistry.msu.com
_contact_crystallographer_name   'Richard Staples'
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id niadp3pna
_olex2_submission_special_instructions 'No special instructions were received'