Three coordination frameworks with copper formate based low dimensional motifs: synthesis, structure and magnetic properties
Bovill, Sally M.; Dixey, Richard J. C.; Saines, Paul J.; CrystEngComm 19 (2017) 1831–; doi:10.1039/C6CE01601D

data_7227816
_publ_section_title
;
 Three coordination frameworks with copper formate based low dimensional
 motifs: synthesis, structure and magnetic properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1831
_journal_paper_doi               10.1039/C6CE01601D
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C15 H19 Cu2 N8 O6, N O3'
_chemical_formula_sum            'C15 H19 Cu2 N9 O9'
_chemical_formula_weight         596.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-01-25 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3812(2)
_cell_length_b                   12.9376(3)
_cell_length_c                   18.1801(4)
_cell_measurement_reflns_used    2876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2206.52(8)
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.02139
_diffrn_orient_matrix_UB_12      -0.10246
_diffrn_orient_matrix_UB_13      0.02018
_diffrn_orient_matrix_UB_21      0.02974
_diffrn_orient_matrix_UB_22      -0.00776
_diffrn_orient_matrix_UB_23      -0.07092
_diffrn_orient_matrix_UB_31      0.04956
_diffrn_orient_matrix_UB_32      0.01413
_diffrn_orient_matrix_UB_33      0.01923
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.468
_diffrn_reflns_theta_min         2.443
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.99
_exptl_absorpt_correction_T_max  1.16
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.747
_refine_diff_density_min         -2.485
_refine_diff_density_rms         0.482
_refine_ls_abs_structure_details
;
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+7.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2334
_reflns_d_resolution_high        0.62
_reflns_d_resolution_low         1.93
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                1998
_reflns_number_total             2637
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            c6ce01601d2.cif
_cod_data_source_block           CuFmIm
_cod_depositor_comments
'Adding full bibliography for 7227816--7227818.cif.'
_cod_database_code               7227816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6-H6A
 0.93 with sigma of 0.01
3. Others
 Fixed Sof: O9(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C1(H1), C9(H9), C8(H8), C7(H7), C2(H2), C5(H5), N5(H5A),
 N2(H2A)

5. The minimum electron density difference is 0.87 A from the Cu atom" 
;
_shelx_res_checksum              59027
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'