Polynuclear ampyrone based 3d coordination clusters
Sampani, Stavroula I.; Loukopoulos, Edward; Azam, Mohammad; Griffiths, Kieran; Abdul-Sada, Alaa; Tizzard, Graham; Coles, Simon; Escuer, Albert; Tsipis, Athanassios; Kostakis, George E.; CrystEngComm 20 (2018) 1411–; doi:10.1039/C7CE02093G

data_7230050
_publ_section_title
;
 Polynuclear ampyrone based 3d coordination clusters
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1411
_journal_paper_doi               10.1039/C7CE02093G
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C23 H25 Cu N3 O4, H2 O'
_chemical_formula_sum            'C23 H27 Cu N3 O5'
_chemical_formula_weight         489.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.444(3)
_cell_angle_beta                 98.421(3)
_cell_angle_gamma                102.838(4)
_cell_formula_units_Z            2
_cell_length_a                   6.8165(3)
_cell_length_b                   12.1809(6)
_cell_length_c                   13.8681(5)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8200
_cell_measurement_theta_min      3.0930
_cell_volume                     1094.80(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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    -27.00  73.00   1.00   15.00    --  -17.00  72.00   0.00  100
  2  \w    -69.00  22.00   1.00   15.00    --  -17.00 -72.00-120.00   91
  3  \w    -68.00  22.00   1.00   15.00    --  -17.00 -72.00  60.00   90
  4  \w    -82.00  -7.00   1.00   15.00    --  -17.00   0.00-120.00   75
  5  \w    -17.00  -1.00   1.00   15.00    --  -17.00  54.00-180.00   16
  6  \w    -80.00  73.00   1.00   15.00    --  -17.00   0.00-150.00  153
  7  \w    -71.00 -38.00   1.00   15.00    --  -17.00 -72.00-180.00   33
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0376209000
_diffrn_orient_matrix_UB_12      0.0601826000
_diffrn_orient_matrix_UB_13      0.0072194000
_diffrn_orient_matrix_UB_21      0.0577947000
_diffrn_orient_matrix_UB_22      -0.0012573000
_diffrn_orient_matrix_UB_23      0.0465602000
_diffrn_orient_matrix_UB_31      0.0837938000
_diffrn_orient_matrix_UB_32      -0.0068609000
_diffrn_orient_matrix_UB_33      -0.0230430000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9202
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75327
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Lath
_exptl_crystal_F_000             510
_exptl_crystal_recrystallization_method
'The material was recrystallised from MeCN as supplied'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         9202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0681P)^2^+1.6711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7361
_reflns_number_total             9202
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9216\% 
 around [0.90 -0.35 -0.27] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           2015ncs0769z_twin1a_hklf4
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_original_cell_volume        1094.80(8)
_cod_database_code               7230050
_chemical_oxdiff_formula         'Cu4 (C18 H16 N3 O2)4 (C5 H9 O2)2 Cl O4'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8235(8) 0.1765(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Free rotating group:
 O101(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              90191
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-01
_olex2_date_sample_submission    2015-12-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id 18SSA(LCOL)Cu(brown)
_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 3.739
_oxdiff_exptl_absorpt_empirical_full_min 0.253
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2