Rare Crystal Structure of Open Spirolactam Ring along with the Closed-Ring Form of a Rhodamine Derivative: Sensing of Cu<sup>2+</sup> Ions from Spinach.
Das, Sujoy; Rissanen, Kari; Sahoo, Prithidipa; ACS omega 4 (2019) 5270–5274; doi:10.1021/acsomega.9b00053

data_4516958
_publ_section_title
;
 Rare Crystal Structure of Open Spirolactam Ring along with the
 Closed-Ring Form of a Rhodamine Derivative: Sensing of Cu<sup>2+</sup>
 Ions from Spinach.
;
_journal_issue                   3
_journal_name_full               'ACS omega'
_journal_page_first              5270
_journal_page_last               5274
_journal_paper_doi               10.1021/acsomega.9b00053
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C41 H43 N5 O4'
_chemical_formula_sum            'C41 H43 N5 O4'
_chemical_formula_weight         669.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                69.231(13)
_cell_angle_beta                 71.022(11)
_cell_angle_gamma                73.095(11)
_cell_formula_units_Z            2
_cell_length_a                   11.256(3)
_cell_length_b                   11.921(3)
_cell_length_c                   15.208(4)
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.24
_cell_volume                     1768.4(8)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.1078
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28170
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        23.099
_diffrn_reflns_theta_max         23.099
_diffrn_reflns_theta_min         1.478
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       cubic
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.083(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.1276
_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^)+(0.1845P)^2^+4.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3169
_refine_ls_wR_factor_ref         0.3579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3225
_reflns_number_total             4987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00053_si_001.cif
_cod_data_source_block           QRA_closed
_cod_database_code               4516958
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N44-C2
 1.45 with sigma of 0.02
 N44-C45
 1.45 with sigma of 0.02
 C43-C1
 1.54 with sigma of 0.02
 C43-C65
 1.54 with sigma of 0.02
 C2-C1AA
 1.54 with sigma of 0.02
 C45-C48
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(N5)
Uanis(C1) = Uanis(C65)
Uanis(C34) = Uanis(C47)
4. Others
 Fixed Sof: H43A(0.6) H43B(0.6) H43C(0.4) H43D(0.4) C65(0.6) H65A(0.6)
 H65B(0.6) H65C(0.6) C1(0.4) H1A(0.4) H1B(0.4) H1C(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B), C39(H39A,H39B), C43(H43A,
 H43B), C43(H43C,H43D), C45(H45A,H45B), C2(H2A,H2B)
5.b Me refined with riding coordinates:
 C41(H41A,H41B,H41C), C48(H48A,H48B,H48C), C65(H65A,H65B,H65C), C1(H1A,H1B,
 H1C), C1AA(H1AA,H1AB,H1AC)
5.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C11(H11), C14(H14), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C34(H34), C36(H36), C37(H37), C38(H38), C42(H42),
  C47(H47)
;
_shelx_res_checksum              57407
_shelx_hkl_checksum              52131
_olex2_submission_special_instructions 'No special instructions were received'