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_1562031
_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_absolute_configuration unk
_chemical_formula_moiety         'C20 H10 Cu3 O19, C10 H11 N3, 2.5(H2 O)'
_chemical_formula_sum            'C30 H26 Cu3 N3 O21.5'
_chemical_formula_weight         963.19
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.315(2)
_cell_angle_beta                 78.168(2)
_cell_angle_gamma                75.064(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9985(11)
_cell_length_b                   9.7296(14)
_cell_length_c                   10.8506(15)
_cell_measurement_reflns_used    5072
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.358
_cell_measurement_theta_min      2.169
_cell_volume                     797.60(19)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0773
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13163
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  0.8779
_exptl_absorpt_correction_T_min  0.6497
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.663
_refine_diff_density_min         -1.729
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                4228
_reflns_number_total             5815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2015-225-222.cif
_cod_data_source_block           p2
_cod_original_formula_sum        'C30 H26 Cu3 N3 O21.50'
_cod_database_code               1562031
_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(O10) = Uanis(Cu3) = Uanis(O19) = Uanis(O3W)
Uanis(C23) = Uanis(N2)
Uanis(O2) = Uanis(O1) = Uanis(O5) = Uanis(O6)
Uanis(O16) = Uanis(O13)
Uanis(C9) = Uanis(C7) = Uanis(C3)
Uanis(O17) = Uanis(O12) = Uanis(O18) = Uanis(C20) = Uanis(C17)
Uanis(C15) = Uanis(C12)
Uanis(C6) = Uanis(C3) = Uanis(C1)
Uanis(O15) = Uanis(O14)
Uanis(C4) = Uanis(C1) = Uanis(C2) = Uanis(C5)
Uanis(C18) = Uanis(C19) = Uanis(C16) = Uanis(C13)
Uanis(C14) = Uanis(C11)
Uanis(C1) = Uanis(C8) = Uanis(O4) = Uanis(O3)
3. Others
 Fixed Sof: O3W(0.5) H3WA(0.5) H3WB(0.5)
 Fixed X: Cu1(0.414749) Cu2(0.161262)
 Fixed Y: Cu1(0.68696) Cu2(0.546069)
 Fixed Z: Cu1(0.823951) Cu2(0.874909)
4.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O19(H19A,H19B),
 O3W(H3WA,H3WB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C12(H12), C15(H15), N1(H1), N2(H2A), N3(H3), C21(H21),
 C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30)
;