Crystal structure of 9-(t-butyl)-3,11-dihydro-6H-pyrazolo [1,5-a]pyrrolo[3′,2′:5,6]pyrido[4,3-d]pyrimidin-6-one hemihydrate, C30H32N10O3
Song, Zhi-Qiang; Hou, Ying-Jie; Sun, Hai-Yang; Zhong, Qi-Di; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 789–791; doi:10.1515/ncrs-2022-0265

data_8107217
_publ_section_title
;
 Crystal structure of 9-(t-butyl)-3,11-dihydro-6H-pyrazolo
 [1,5-a]pyrrolo[3&#x2032;,2&#x2032;:5,6]pyrido[4,3-d]pyrimidin-6-one
 hemihydrate, C30H32N10O3
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              789
_journal_page_last               791
_journal_paper_doi               10.1515/ncrs-2022-0265
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         '2(C15 H15 N5 O), H2 O'
_chemical_formula_sum            'C30 H32 N10 O3'
_chemical_formula_weight         580.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 113.001(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.447(2)
_cell_length_b                   20.130(4)
_cell_length_c                   14.772(3)
_cell_measurement_reflns_used    2323
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      21.99
_cell_measurement_theta_min      2.35
_cell_volume                     2859.5(10)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16503
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         1.807
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0042(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0781P)^2^+0.0509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3552
_reflns_number_total             5904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0265_suppl.cif
_cod_data_source_block           k6-1
_cod_original_cell_volume        2859.7(10)
_cod_database_code               8107217
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C27 \\sim C30A \\sim C27 \\sim C28A \\sim C27 \\sim C29B \\sim C27 \\sim C29A
\\sim C27 \\sim C28B \\sim C27 \\sim C30B: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
3. Others
 Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
4.a Riding coordinates:
 O3(H3A,H3B), C29B(H29D,H29E,H29F)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N1(H1), C10(H10), C2(H2), C1(H1A), C5(H5), N6(H6), C16(H16)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C28A(H28A,H28B,
 H28C), C30A(H30A,H30B,H30C), C29A(H29A,H29B,H29C), C30B(H30D,H30E,H30F),
 C28B(H28D,H28E,H28F)
;
_olex2_submission_special_instructions 'No special instructions were received'