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_4516957
_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         '2(Cl O4), C41 H44 N5 O4, 2(H2 O)'
_chemical_formula_sum            'C41 H48 Cl2 N5 O14'
_chemical_formula_weight         905.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.467(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.698(6)
_cell_length_b                   19.777(8)
_cell_length_c                   15.179(6)
_cell_measurement_reflns_used    5777
_cell_measurement_temperature    296(2)
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_cell_measurement_theta_min      2.29
_cell_volume                     4384(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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1014
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.463
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.26
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_exptl_crystal_size_min          0.1
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_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7706
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_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1331P)^2^+5.8677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4402
_reflns_number_total             7706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00053_si_002.cif
_cod_data_source_block           QRA_open
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4516957
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl01-O01B
 1.45 with sigma of 0.02
 Cl01-O01I
 1.45 with sigma of 0.02
 Cl01-O2AA
 1.45 with sigma of 0.02
 Cl01-O01H
 1.45 with sigma of 0.02
 N011-C0AA
 1.525 with sigma of 0.02
 C0AA-C1
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C01L) = Uanis(C0AA)
Uanis(C1) = Uanis(C01N)
4. Others
 Fixed Sof: Cl(0.85) C01L(0.6) H01W(0.6) H01X(0.6) C01N(0.6) H01Y(0.6) H(0.6)
 HA(0.6) C1(0.4) H1A(0.4) H1B(0.4) H1C(0.4) C0AA(0.4) H0AA(0.4) H0AB(0.4)
 O1(0.5) O2(0.5) O0AA(0.5) O4(0.25) O1AA(0.5) Cl1(0.15) O3AA(0.25) O4AA(0.25)
 O5AA(0.25) O8AA(0.25) O9AA(0.25) O8(0.25) O5(0.25)
5.a Free rotating group:
 O00H(H00C,H00D), O00Q(H00E,H00F)
5.b Secondary CH2 refined with riding coordinates:
 C00X(H00A,H00B), C010(H01A,H01B), C013(H01C,H01D), C016(H01E,H01F), C017(H01G,
 H01H), C01A(H01I,H01J), C01L(H01W,H01X), C0AA(H0AA,H0AB)
5.c Aromatic/amide H refined with riding coordinates:
 N006(H006), N008(H008), C00J(H00J), C00K(H00K), C00M(H00M), C00N(H00N),
 C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C015(H015), C018(H018), C019(H019), C01C(H01K), C01D(H01L), C01E(H01M)
5.d Idealised Me refined as rotating group:
 C01G(H01N,H01O,H01P), C01J(H01Q,H01R,H01S), C01K(H01T,H01U,H01V), C01N(H01Y,H,
 HA), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              50123
_shelx_hkl_checksum              36934
_olex2_submission_special_instructions 'No special instructions were received'