Directed synthesis of {CuZn} and {CuZn} heterometallic complexes.
Heras Ojea, María José; Wilson, Claire; Coles, Simon J.; Tuna, Floriana; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19275–19281; doi:10.1039/c5dt03344f

data_1540033
_publ_section_title
;
 Directed synthesis of {CuZn} and {CuZn} heterometallic complexes.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19275
_journal_page_last               19281
_journal_paper_doi               10.1039/c5dt03344f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C88 H200 Cl3 Cu8 N16 O68 Zn8, 2(Cl), 3(Cl O4), 16(H2O)'
_chemical_formula_sum            'C88 H232 Cl8 Cu8 N16 O96 Zn8'
_chemical_formula_weight         4365.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-19
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
;
2015-07-29 deposited with the CCDC.
2015-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.5574(19)
_cell_length_b                   26.5574(19)
_cell_length_c                   13.1186(10)
_cell_measurement_reflns_used    20855
_cell_measurement_temperature    100
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_cell_measurement_theta_min      2.2
_cell_volume                     9252.5(12)
_computing_cell_refinement
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CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
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_computing_data_collection
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CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
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CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
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_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
scan:
    Number of images: 123
               Slice: -50.0000 - 73.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 43.0000
                 Phi: -78.0000
                 XTD: 44.9137
              2theta: -17.0831
scan:
    Number of images: 22
               Slice: -49.0000 - -27.0000
         Image width: 1.0000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 14.0000
                 Phi: 128.0000
                 XTD: 44.9137
              2theta: -17.0831
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.037279
_diffrn_orient_matrix_UB_12      0.001319
_diffrn_orient_matrix_UB_13      -0.005133
_diffrn_orient_matrix_UB_21      0.003584
_diffrn_orient_matrix_UB_22      -0.033141
_diffrn_orient_matrix_UB_23      0.017512
_diffrn_orient_matrix_UB_31      -0.007904
_diffrn_orient_matrix_UB_32      -0.036087
_diffrn_orient_matrix_UB_33      -0.066678
_diffrn_radiation_collimation    'Confocal mirrors, HF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1349
_diffrn_reflns_av_unetI/netI     0.1495
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23159
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.182
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1522
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1373P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4716
_reflns_number_total             8104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03344f2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-12

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1540032--1540033.cif.
;
_cod_original_cell_volume        9252.5(15)
_cod_database_code               1540033
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,H) groups, All
  N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-H1 = O2-H2
 0.84 with sigma of 0.02
 O71X-C71A \\sim O71A-C71A \\sim O71Y-C71A
 with sigma of 0.02
 O5C-O6C \\sim O5C-O7C \\sim O5C-O8C \\sim O6C-O7C \\sim O6C-O8C \\sim O7C-O8C
 with sigma of 0.02
 O1C-O2C \\sim O1C-O3C \\sim O1C-O4C \\sim O2C-O3C \\sim O2C-O4C \\sim O3C-O4C
 with sigma of 0.02
 Cl4C-O5C \\sim Cl4C-O6C \\sim Cl4C-O7C \\sim Cl4C-O8C \\sim Cl3C-O1C \\sim
Cl3C-O2C \\sim Cl3C-O4C ~
 Cl3C-O3C
 with sigma of 0.02
 O11X-C11B \\sim O11B-C11B \\sim O72X-C72B \\sim O72B-C72B
 with sigma of 0.02
3. Others
 Sof(Cl2A)=0.25*(1-FVAR(2))
 Sof(Cl2)=0.25*FVAR(2)
 Uiso(O5C)=Uiso(O6C)=Uiso(O7C)=Uiso(O8C)=FVAR(2)
 Fixed Sof: O71A(0.6) H71A(0.6) H71B(0.6) H71C(0.6) H71D(0.2) H71E(0.2)
 H71F(0.2) H71G(0.2) O11B(0.75) H11D(0.75) O72B(0.8) H72C(0.8) H11E(0.75)
 H11F(0.75) H11G(0.25) H11H(0.25) H72D(0.8) H72E(0.8) H72F(0.2) H72G(0.2)
 O11X(0.25) H11X(0.25) O71X(0.2) H71X(0.2) O72X(0.2) H72X(0.2) O71Y(0.2)
 H71Y(0.2) Cl3C(0.75) O1C(0.75) O2C(0.75) O3C(0.75) O4C(0.75) Cl4C(0.75)
 O5C(0.75) O6C(0.75) O7C(0.75) O8C(0.75) O1W(0.5) O4W(0.5)
4.a Ternary CH refined with riding coordinates:
 N2A(H2A), N6A(H6A), N2B(H2B), N6B(H6B)
4.b Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C10A(H10B,H10C), C11A(H11B,
 H11C), C12A(H12A,H12B), C71A(H71B,H71C), C71A(H71D,H71E), C71A(H71F,H71G),
 C72A(H72A,H72B), C73A(H73B,H73C), C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,
 H5BB), C10B(H10D,H10E), C11B(H11E,H11F), C11B(H11G,H11H), C12B(H12D,H12E),
 C71B(H71H,H71I), C72B(H72D,H72E), C72B(H72F,H72G), C73B(H73E,H73F)
4.c Tetrahedral OH refined with riding coordinates:
 O71A(H71A), O11B(H11D), O72B(H72C), O11X(H11X), O71X(H71X), O72X(H72X),
 O71Y(H71Y)
4.d Idealised tetrahedral OH refined as rotating group:
 O10A(H10A), O11A(H11A), O73A(H73A), O12B(H12C), O73B(H73D)
;
_shelx_res_checksum              71754
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'