Crystal structure of (2,2′-((naphthalen-1-ylmethyl)azanediyl)diacetato-κ3 N,O,O′)-(1,10-phenanthroline-κ2 N,N′)-copper(II) trihydrate, CuC27H27N3O7
Xu, Xingman; Sun, Renqiang; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 417–419; doi:10.1515/ncrs-2022-0050

data_8105712
_publ_section_title
;
 Crystal structure of
 (2,2&#x2032;-((naphthalen-1-ylmethyl)azanediyl)diacetato-\k3
 N,O,O&#x2032;)-(1,10-phenanthroline-\k2 N,N&#x2032;)-copper(II)
 trihydrate, CuC27H27N3O7
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              417
_journal_page_last               419
_journal_paper_doi               10.1515/ncrs-2022-0050
_journal_volume                  237
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H21 Cu N3 O4, 3(H2 O)'
_chemical_formula_sum            'C27 H27 Cu N3 O7'
_chemical_formula_weight         569.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9142(18)
_cell_length_b                   7.3271(6)
_cell_length_c                   14.7386(11)
_cell_measurement_reflns_used    4499
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.76
_cell_volume                     2474.5(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2003) [1]'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2003)'
_computing_molecular_graphics    'Diamond (Brandenburg, 2006)[5]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[5]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [2-3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2015) [2-3]'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16736
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         1.777
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.8975
_exptl_absorpt_correction_T_min  0.7056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2008) [6]'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
; 
 Flack x determined using 1386 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.033(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0467P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.835
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                4224
_reflns_number_total             5352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0050_suppl.cif
_cod_data_source_block           2
_cod_database_code               8105712
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.896
_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 O(H,H) groups 
2.a Free rotating group: 
 O5(H5C,H5D), O6(H6A,H6B), O7(H7A,H7B) 
2.b Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B) 
2.c Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), 
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25) 
;
_olex2_submission_special_instructions 'No special instructions were received'