A bis-copper(II)‒[<small>D</small>-βVal^3,7^]ascidiacyclamide complex enveloping two square pyramids and sharing an apex atom from a carbonate anion
Asano, Akiko; Doi, Mitsinobu; Acta Crystallographica Section C 75 (2019) 1182–1187; doi:10.1107/S2053229619007952

data_2021734
_publ_section_title
;
 A bis-copper(II)--[<small>D</small>-\bVal^3,7^]ascidiacyclamide complex
 enveloping two square pyramids and sharing an apex atom from a carbonate
 anion
;
_journal_coeditor_code           CU3139
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1182
_journal_page_last               1187
_journal_paper_doi               10.1107/S2053229619007952
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_compound_source        synthesis
_chemical_formula_iupac
'[Cu2 (C O3) (C38 H54 N8 O6 S2) (H2 O1)], H2 O'
_chemical_formula_moiety         'C39 H56 Cu2 N8 O10 S2, H2 O'
_chemical_formula_sum            'C39 H58 Cu2 N8 O11 S2'
_chemical_formula_weight         1006.13
_chemical_name_systematic
;
[[<i>D</i>-\bVal^3,7^]Ascidiacyclamide(2-)]aqua-\m-carbonato-dicopper(II)
monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 113.077(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6321(17)
_cell_length_b                   13.9512(19)
_cell_length_c                   14.792(2)
_cell_measurement_reflns_used    6711
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.28
_cell_volume                     2398.2(6)
_computing_cell_refinement
;
SMART (Bruker, 1998)
;
_computing_data_collection
;
SMART (Bruker, 1998)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 1998)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      240(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.1291
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13331
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.496
_diffrn_source                   'M18XCE rotating anode'
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       needle
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.006
_refine_diff_density_min         -1.985
_refine_ls_abs_structure_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8140
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1145
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2753
_refine_ls_wR_factor_ref         0.2832
_reflns_number_gt                5984
_reflns_number_total             8140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3139sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2398.3(6)
_cod_database_code               2021734
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.860
_shelx_hkl_checksum              66730
_shelx_res_checksum              86853
_cod_database_fobs_code 2021734