Structure and properties of a novel staircase-like decanuclear [CuII10] cluster supported by carbonate and carboxylate bridges
Haldar, Shobhraj; Vijaykumar, Gonela; Carrella, Luca; Musie, Ghezai T.; Bera, Manindranath; New Journal of Chemistry 42 (2018) 1276–; doi:10.1039/C7NJ03714G

data_7056760
_publ_section_title
;
 Structure and properties of a novel staircase-like decanuclear [CuII10]
 cluster supported by carbonate and carboxylate bridges
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1276
_journal_paper_doi               10.1039/C7NJ03714G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'2(C65 H62 Cu5 N8 O17), 7.83(H2 O), 3.33(C H4 O)'
_chemical_formula_sum            'C133.33 H152.98 Cu10 N16 O45.16'
_chemical_formula_weight         3337.74
_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
_audit_creation_date             2016-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-08-04 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.086(4)
_cell_angle_beta                 84.022(4)
_cell_angle_gamma                69.942(5)
_cell_formula_units_Z            1
_cell_length_a                   12.9346(7)
_cell_length_b                   16.1294(9)
_cell_length_c                   18.8407(9)
_cell_measurement_reflns_used    8677
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7730
_cell_measurement_theta_min      1.7420
_cell_volume                     3670.0(4)
_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    'SIR-97/(Altomare, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26348
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1701
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   0.675
_exptl_transmission_factor_min   0.492
_platon_squeeze_details
;
;
_refine_diff_density_max         2.557
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         15980
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0656P)^2^+21.5432P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12832
_reflns_number_total             15980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03714g2.cif
_cod_data_source_block           Cu10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7056760.cif.
;
_cod_original_cell_volume        3669.9(4)
_cod_database_code               7056760
_shelxl_version_number           2012-9
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O17-H17
 0.85 with sigma of 0.01
 C65-H17
 1.853717 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C67) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O19(0.66667) H19(0.66667) O23(0.33333) O24(0.5) O25(0.25)
 C67(0.66667) H67A(0.66667) H67B(0.66667) H67C(0.66667) O26(0.5) O22(0.33333)
5.a Riding coordinates:
 O19(H19)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C32(H32)
5.c Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C34(H34A,H34B), C33(H33A,H33B), C3(H3A,H3B), C35(H35A,H35B),
 C2(H2A,H2B), C12(H12A,H12B), C4(H4A,H4B), C43(H43A,H43B), C49(H49A,H49B),
 C57(H57A,H57B), C18(H18A,H18B)
5.d Aromatic/amide H refined with riding coordinates:
 C29(H29), C21(H21), C9(H9), C47(H47), C7(H7), C53(H53), C23(H23), C30(H30),
 C20(H20), C61(H61), C6(H6), C28(H28), C37(H37), C51(H51), C54(H54), C62(H62),
 C40(H40), C14(H14), C31(H31), C52(H52), C46(H46), C22(H22), C16(H16), C8(H8),
 C38(H38), C45(H45), C39(H39), C48(H48), C59(H59), C17(H17A), C15(H15), C60(H60)
5.e Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
5.f Idealised tetrahedral OH refined as rotating group:
 O18(H18)
;
_shelx_res_checksum              268
_olex2_submission_special_instructions 'No special instructions were received'