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_1540032
_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
'C13 H27 Cl Cu N2 O8 Zn, C13 H25 Cl Cu N2 O8 Zn, 2.5(C O), 0.5(O)'
_chemical_formula_sum            'C28.5 H63 Cl2 Cu2 N4 O19 Zn2'
_chemical_formula_weight         1094.55
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-09-24 deposited with the CCDC.
2015-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                109.186(7)
_cell_angle_beta                 90.177(7)
_cell_angle_gamma                108.009(7)
_cell_formula_units_Z            2
_cell_length_a                   10.9593(12)
_cell_length_b                   13.8454(15)
_cell_length_c                   17.4039(19)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.20
_cell_volume                     2355.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1507
_diffrn_reflns_av_unetI/netI     0.2078
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44970
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       plate
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.530
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         44970
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.2216
_refine_ls_R_factor_gt           0.1284
_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^)+(0.1687P)^2^+43.4739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3062
_refine_ls_wR_factor_ref         0.3782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22628
_reflns_number_total             44970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03344f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-12

 Adding full bibliography for 1540032--1540033.cif.
;
_cod_original_formula_sum        'C28.50 H63 Cl2 Cu2 N4 O19 Zn2'
_cod_database_code               1540032
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.860(8) 0.140(8)
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) groups
3. Restrained distances
 O3S-C3S = O2S-C2S = O1S-C1S
 1.41 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O3S(0.5) C3S(0.5) O4S(0.5)
6.a Ternary CH refined with riding coordinates:
 N101(H101), N102(H102), N201(H201), N202(H202)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C104(H10E,H10F), C105(H10G,H10H), C106(H10I,
 H10J), C107(H10K,H10L), C109(H10M,H10N), C110(H11A,H11B), C111(H11C,H11D),
 C201(H20A,H20B), C202(H20C,H20D), C205(H20E,H20F), C206(H20G,H20H), C207(H20I,
 H20J), C209(H20K,H20L), C211(H21A,H21B)
6.c Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
6.d Aromatic/amide H refined with riding coordinates:
 C204(H204), C210(H210)
6.e Idealised tetrahedral OH refined as rotating group:
 O105(H105), O106(H106), O109(H109), O111(H111), O205(H205), O206(H206),
 O209(H209), O211(H211)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'