Influence of water on the structure and magnetic properties of a copper bromide coordination compound with 3-amino-4-ethoxycarbonylpyrazole
Berezin, A. S.; Ivanova, A. D.; Komarov, V. Yu.; Nadolinny, V. A.; Lavrenova, L. G.; New Journal of Chemistry 42 (2018) 4902–; doi:10.1039/C8NJ00017D

data_7057017
_publ_section_title
;
 Influence of water on the structure and magnetic properties of a copper
 bromide coordination compound with 3-amino-4-ethoxycarbonylpyrazole
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4902
_journal_paper_doi               10.1039/C8NJ00017D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C24 H36 Br Cu N12 O8 1+, Br 1-, H2O'
_chemical_formula_sum            'C24 H38 Br2 Cu N12 O9'
_chemical_formula_weight         862.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-07 deposited with the CCDC.
2018-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.075(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.7828(17)
_cell_length_b                   5.6317(3)
_cell_length_c                   20.8991(12)
_cell_measurement_reflns_used    7875
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.19
_cell_volume                     3567.2(3)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.874
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.916
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0709 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.7786. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       plank
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.376(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8500
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0816
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6714
_reflns_number_total             8500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00017d2.cif
_cod_data_source_block           structure2
_cod_depositor_comments
'Adding full bibliography for 7057015--7057017.cif.'
_cod_database_code               7057017
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.297
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.624(10)
 0.376(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B), C35(H35A,H35B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N22(H22), N32(H32), N42(H42), C11(H11), C21(H21), C31(H31), C41(H41)
3.c X=CH2 refined with riding coordinates:
 N13(H13A,H13B), N23(H23A,H23B), N33(H33A,H33B), N43(H43A,H43B)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              19650
_olex2_submission_special_instructions 'No special instructions were received'