Temperature-dependent polymorphism and magnetic properties of three-dimensional copper pyromellitate coordination polymers containing 4,4′-dipyridylamine
Mizzi, Jessica E.; Staples, Richard J.; LaDuca, Robert L.; Journal of Solid State Chemistry 225 (2015) 222–230; doi:10.1016/j.jssc.2014.12.021

data_1562030
_publ_section_title
;
 Temperature-dependent polymorphism and magnetic properties of
 three-dimensional copper pyromellitate coordination polymers containing
 4,4&#x2032;-dipyridylamine
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              222
_journal_page_last               230
_journal_paper_doi               10.1016/j.jssc.2014.12.021
_journal_volume                  225
_journal_year                    2015
_chemical_formula_moiety         'C60 H42 Cu3 N12 O16, 3(H2 O)'
_chemical_formula_sum            'C60 H48 Cu3 N12 O19'
_chemical_formula_weight         1431.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                94.475(2)
_cell_angle_beta                 96.731(2)
_cell_angle_gamma                106.684(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3201(13)
_cell_length_b                   10.8466(14)
_cell_length_c                   12.7508(17)
_cell_measurement_reflns_used    5263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.891
_cell_measurement_theta_min      2.402
_cell_volume                     1348.4(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.998
_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_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.865
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20011
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.984
_diffrn_reflns_theta_min         1.619
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0705 before and 0.0624 after correction.
The Ratio of minimum to maximum transmission is 0.9314.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             731
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         4228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0409P)^2^+2.3137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3111
_reflns_number_total             4228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2015-225-222.cif
_cod_data_source_block           p1
_cod_database_code               1562030
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C27)
3. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5)
4.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N5(H5), N2(H2), C12(H12), C1(H1), C11(H11), C26(H26), C6(H6A),
 C17(H17), C10(H10), C20(H20), C7(H7), C5(H5A), C16(H16), C19(H19), C23(H23),
 C4(H4), C9(H9), C14(H14), C2(H2A), C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'