Hydrothermal synthesis and crystal structure of poly[bis(μ2-3-(3,5-dicarboxyphenoxy)phthalato-κ3 O,O′:O′′)-(μ2-1,2-di(pyridin-4-yl)ethane-κ2 N:N′)copper(II)], C22H14CuNO9
Yun-Ping, Li; Feng-Yang, Ju; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 387–389; doi:10.1515/ncrs-2017-0281

data_8106161
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of
 poly[bis(\m2-3-(3,5-dicarboxyphenoxy)phthalato-\k3
 O,O&#x2032;:O&#x2032;&#x2032;)-(\m2-1,2-di(pyridin-4-yl)ethane-\k2
 N:N&#x2032;)copper(II)], C22H14CuNO9
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              387
_journal_page_last               389
_journal_paper_doi               10.1515/ncrs-2017-0281
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C22 H14 Cu N O9'
_chemical_formula_sum            'C22 H14 Cu N O9'
_chemical_formula_weight         499.88
_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   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                72.719(4)
_cell_angle_beta                 79.598(5)
_cell_angle_gamma                85.190(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9208(4)
_cell_length_b                   10.2954(4)
_cell_length_c                   13.1361(7)
_cell_measurement_reflns_used    4249
_cell_measurement_temperature    264(1)
_cell_measurement_theta_max      26.4650
_cell_measurement_theta_min      4.1000
_cell_volume                     1005.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      264(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8518
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -20.00  26.00   1.00    9.99    --  -12.69 -99.00 -30.00   46
  2  \w    -29.00  55.00   1.00    9.99    --  -12.69  57.00-180.00   84
  3  \w     -3.00  81.00   1.00    9.99    --   13.62  57.00  60.00   84
  4  \w    -54.00  30.00   1.00    9.99    --   13.62 -57.00 -60.00   84
  5  \w     -3.00  81.00   1.00    9.99    --   13.62  57.00 150.00   84
  6  \w     -3.00  81.00   1.00    9.99    --   13.62  57.00 -90.00   84
  7  \w    -85.00 -34.00   1.00    9.99    --  -12.69 178.00 -30.00   51
  8  \w    -20.00  15.00   1.00    9.99    --   13.62 -99.00  90.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0402673000
_diffrn_orient_matrix_UB_12      0.0233812000
_diffrn_orient_matrix_UB_13      0.0350304000
_diffrn_orient_matrix_UB_21      -0.0817057000
_diffrn_orient_matrix_UB_22      0.0134983000
_diffrn_orient_matrix_UB_23      0.0280450000
_diffrn_orient_matrix_UB_31      0.0007503000
_diffrn_orient_matrix_UB_32      -0.0669511000
_diffrn_orient_matrix_UB_33      0.0356660000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10787
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0414P)^2^+1.0725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3252
_reflns_number_total             3680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0281_suppl.cif
_cod_data_source_block           a
_cod_database_code               8106161
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C1(H1), C18(H18), C20(H20), C2(H2), C5(H5), C4(H4), C12(H12),
 C10(H10), C11(H11)
2.c Idealised tetrahedral OH refined as rotating group:
 O9(H9), O7(H7)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.774