The crystal structure of bis(N,N-dimethylformamide-κO)-tetrakis(9H-xanthene-9-carboxylic-carboxylate-κ2 O:O′)dicopper(II) - acetonitrile (1/2), C66H56Cu2N4O14
Ren-Shu, Wang; Jing, Feng; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 453–454; doi:10.1515/ncrs-2018-0464

data_8105679
_publ_section_title
;
 The crystal structure of
 bis(N,N-dimethylformamide-\kO)-tetrakis(9H-xanthene-9-carboxylic-carboxylate-\k2
 O:O&#x2032;)dicopper(II) - acetonitrile (1/2), C66H56Cu2N4O14
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              453
_journal_page_last               454
_journal_paper_doi               10.1515/ncrs-2018-0464
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C31 H25 Cu N O7, C2 H3 N'
_chemical_formula_sum            'C33 H28 Cu N2 O7'
_chemical_formula_weight         628.11
_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                77.782(4)
_cell_angle_beta                 86.304(4)
_cell_angle_gamma                69.491(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0791(5)
_cell_length_b                   11.5747(5)
_cell_length_c                   12.4037(6)
_cell_measurement_reflns_used    5210
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5600
_cell_measurement_theta_min      2.9820
_cell_volume                     1455.97(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1213
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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     -4.00  83.00   1.00    5.79    --   15.49  77.00 -90.00   87
  2  \w     20.00  47.00   1.00    5.79    --  -16.12  77.00 -90.00   27
  3  \w     12.00  51.00   1.00    5.79    --  -16.12  77.00-180.00   39
  4  \w    -43.00  21.00   1.00    5.79    --  -16.12  77.00   0.00   64
  5  \w    -31.00  24.00   1.00    5.79    --  -16.12  77.00  60.00   55
  6  \w    -11.00  83.00   1.00    5.79    --   15.49  77.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0510327000
_diffrn_orient_matrix_UB_12      0.0074068000
_diffrn_orient_matrix_UB_13      -0.0351112000
_diffrn_orient_matrix_UB_21      -0.0147778000
_diffrn_orient_matrix_UB_22      -0.0338995000
_diffrn_orient_matrix_UB_23      -0.0355765000
_diffrn_orient_matrix_UB_31      -0.0430128000
_diffrn_orient_matrix_UB_32      0.0570904000
_diffrn_orient_matrix_UB_33      -0.0304190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6227
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0326P)^2^+0.3072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5277
_reflns_number_total             6227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0464_suppl.cif
_cod_data_source_block           exp_5946
_cod_database_code               8105679
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.843
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O7, C29
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C3(H3), C18(H18), C19(H19), C12(H12), C9(H9), C6(H6), C5(H5),
 C27(H27), C10(H10), C11(H11), C4(H4), C24(H24), C21(H21), C20(H20), C25(H25),
 C26(H26)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C)
;