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_7230053
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C29 H23 Cu N3 O4), C6 H16 N, Cl O4, H2 O'
_chemical_formula_sum            'C64 H64 Cl Cu2 N7 O13'
_chemical_formula_weight         1301.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4231(4)
_cell_length_b                   30.1689(9)
_cell_length_c                   14.2158(4)
_cell_measurement_reflns_used    19912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1410
_cell_measurement_theta_min      2.4450
_cell_volume                     5756.8(3)
_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 0.999
_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   -107.00  22.00   1.00   90.00    --  -17.00 -72.00 120.00  129
  2  \w    -97.00  12.00   1.00   90.00    --  -17.00 -36.00 -30.00  109
  3  \w   -107.00  22.00   1.00   90.00    --  -17.00 -72.00  90.00  129
  4  \w    -99.00  15.00   1.00   90.00    --  -17.00 -36.00 -60.00  114
  5  \w   -107.00 -91.00   1.00   90.00    --  -17.00 -72.00 150.00   16
;
_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      -0.0029894000
_diffrn_orient_matrix_UB_12      0.0234787000
_diffrn_orient_matrix_UB_13      0.0004611000
_diffrn_orient_matrix_UB_21      0.0527070000
_diffrn_orient_matrix_UB_22      0.0013201000
_diffrn_orient_matrix_UB_23      -0.0018218000
_diffrn_orient_matrix_UB_31      -0.0019852000
_diffrn_orient_matrix_UB_32      0.0001528000
_diffrn_orient_matrix_UB_33      -0.0498607000
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            56032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.193
_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    0.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38458
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       blade
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
'The material was recrystallised from MeCN as supplied'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         10159
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0789P)^2^+14.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8454
_reflns_number_total             10159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce02093g2.cif
_cod_data_source_block           2015ncs0766r1y
_cod_depositor_comments
'Adding full bibliography for 7230048--7230057.cif.'
_cod_database_code               7230053
_chemical_oxdiff_formula         C64H61ClCu2N7O13
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.96(2) 0.04(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O303-H40A
 2.02 with sigma of 0.02
 H40B-O101
 2.13 with sigma of 0.02
4. Rigid body (RIGU) restrains
 N201, H201, C201, H20A, H20B, C202, H20C, H20D, H20E, C203, H20F, H20G, C204,
 H20H, H20I, H20J, C205, H20K, H20L, C206, H20M, H20N, H20O
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Free rotating group:
 O401(H40A,H40B)
5.b Ternary CH refined with riding coordinates:
 N201(H201)
5.c Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C203(H20F,H20G), C205(H20K,H20L)
5.d 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), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C102(H102), C103(H103), C104(H104), C105(H105), C107(H107),
 C114(H114), C115(H115), C116(H116), C117(H117), C118(H118), C121(H121),
 C122(H122), C123(H123), C125(H125), C126(H126), C127(H127), C128(H128)
5.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C111(H11D,H11E,H11F), C112(H11G,
 H11H,H11I), C202(H20C,H20D,H20E), C204(H20H,H20I,H20J), C206(H20M,H20N,H20O)
;
_shelx_res_checksum              36491
_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 12SSE(LCOL)
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.156
_oxdiff_exptl_absorpt_empirical_full_min 0.589